# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p-1
_database_code_depnum_ccdc_archive 'CCDC 1894388'
loop_
_audit_author_name
_audit_author_address
'Dae Young Bae'
;Pohang University of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_p-1                 
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 7.0 Ratio
RESPONSE: This alert results from the disorder on the isopropyl groups. 
It is unremarkable for the methyl carbon atoms of isopropyl groups to show moderate rotolibrations. 
This leads larger Ueq values for those carbon atoms than rigidly bound carbon atoms. 
This does not mean incorrect atomic identification even though the methyl carbon atoms on the isopropyl groups show high Ueq values.
;
# end Validation Reply Form
_audit_creation_date             2019-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C70 H92 Cr N O4'
_chemical_formula_sum            'C72.50 H98 Cr N O4'
_chemical_formula_weight         1099.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1640(11)
_cell_length_b                   14.4132(11)
_cell_length_c                   18.4865(14)
_cell_angle_alpha                108.161(3)
_cell_angle_beta                 91.379(3)
_cell_angle_gamma                110.604(3)
_cell_volume                     3318.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    108134
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.173
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.968
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            108134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.173
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10052
_reflns_number_total             11295
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11295
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0655P)²+3.1562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1369
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.05
3. Others
 Sof(H29A)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(H29)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Fixed Sof: H7A(0.5) H7B(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C9B(0.5)
 H9BA(0.5) H9BB(0.5) H9BC(0.5)
4.a Ternary CH refined with riding coordinates:
 C54(H54), C13(H13), C32(H32), C35(H35), C57(H57), C10(H10), C51(H51),
 C29(H29), C29(H29A), C7(H7A), C7(H7B)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C22(H22A,H22B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,
 H69B), C70(H70A,H70B), C68(H68A,H68B)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C43(H43), C63(H63), C61(H61), C18(H18), C41(H41), C62(H62),
 C17(H17), C42(H42), C28(H28), C50(H50), C46(H46), C24(H24), C2(H2), C6(H6)
4.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,
 H59C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C58(H58A,H58B,H58C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C8(H8A,H8B,H8C), C30(H30A,H30B,H30C),
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C52(H52A,H52B,H52C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C31A(H31A,H31B,H31C), C31(H31D,H31E,H31F),
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.67919(2) 0.36757(2) 0.81176(2) 0.02315(10) Uani 1 1 d . . . . .
O1 O 0.81466(10) 0.37861(11) 0.80542(8) 0.0292(3) Uani 1 1 d . . . . .
O3 O 0.56491(11) 0.30437(11) 0.85514(8) 0.0320(3) Uani 1 1 d . . . . .
O2 O 0.64156(12) 0.42259(11) 0.74258(8) 0.0336(3) Uani 1 1 d . . . . .
O5 O 0.63622(11) 0.22414(11) 0.72650(8) 0.0336(3) Uani 1 1 d . . . . .
N1 N 0.72708(12) 0.50959(12) 0.90202(9) 0.0213(3) Uani 1 1 d . . . . .
C64 C 0.60023(15) 0.43323(16) 0.98006(11) 0.0257(4) Uani 1 1 d . . . . .
C65 C 0.56270(15) 0.32786(16) 0.93094(11) 0.0256(4) Uani 1 1 d . . . . .
C39 C 0.63436(15) 0.51604(15) 0.75377(11) 0.0248(4) Uani 1 1 d . . . . .
C40 C 0.68906(15) 0.60477(15) 0.81824(11) 0.0247(4) Uani 1 1 d . . . . .
C20 C 0.90821(15) 0.52097(16) 0.91984(11) 0.0255(4) Uani 1 1 d . . . . .
C38 C 0.57081(15) 0.52423(16) 0.69815(11) 0.0269(4) Uani 1 1 d . . . . .
C21 C 0.90392(15) 0.45192(15) 0.84621(11) 0.0252(4) Uani 1 1 d . . . . .
C44 C 0.76536(15) 0.60036(15) 0.87352(11) 0.0245(4) Uani 1 1 d . . . . .
H44A H 0.8253 0.5972 0.8480 0.029 Uiso 1 1 calc R . . . .
H44B H 0.7887 0.6666 0.9184 0.029 Uiso 1 1 calc R . . . .
C16 C 0.99390(15) 0.45770(17) 0.81409(12) 0.0290(4) Uani 1 1 d . . . . .
C60 C 0.52360(15) 0.24602(16) 0.96144(12) 0.0279(4) Uani 1 1 d . . . . .
C19 C 1.00212(16) 0.59464(17) 0.96126(12) 0.0297(4) Uani 1 1 d . . . . .
H19 H 1.0051 0.6417 1.0112 0.036 Uiso 1 1 calc R . . . .
C22 C 0.81197(15) 0.51321(16) 0.95453(11) 0.0262(4) Uani 1 1 d . . . . .
H22A H 0.7883 0.4488 0.9688 0.031 Uiso 1 1 calc R . . . .
H22B H 0.8276 0.5747 1.0024 0.031 Uiso 1 1 calc R . . . .
C43 C 0.56410(16) 0.62111(17) 0.70869(13) 0.0332(5) Uani 1 1 d . . . . .
H43 H 0.5222 0.6275 0.6711 0.040 Uiso 1 1 calc R . . . .
C63 C 0.59848(16) 0.45654(17) 1.05875(12) 0.0306(5) Uani 1 1 d . . . . .
H63 H 0.6247 0.5280 1.0921 0.037 Uiso 1 1 calc R . . . .
C66 C 0.64088(15) 0.51815(15) 0.94574(11) 0.0253(4) Uani 1 1 d . . . . .
H66A H 0.6648 0.5877 0.9875 0.030 Uiso 1 1 calc R . . . .
H66B H 0.5849 0.5147 0.9106 0.030 Uiso 1 1 calc R . . . .
C61 C 0.52204(16) 0.27281(17) 1.04048(12) 0.0318(5) Uani 1 1 d . . . . .
H61 H 0.4949 0.2183 1.0615 0.038 Uiso 1 1 calc R . . . .
C18 C 1.09146(16) 0.60025(17) 0.93053(12) 0.0317(5) Uani 1 1 d . . . . .
H18 H 1.1553 0.6507 0.9593 0.038 Uiso 1 1 calc R . . . .
C41 C 0.67852(16) 0.69992(16) 0.82719(13) 0.0305(4) Uani 1 1 d . . . . .
H41 H 0.7142 0.7598 0.8715 0.037 Uiso 1 1 calc R . . . .
C47 C 0.55105(16) 0.07638(16) 0.90927(12) 0.0310(5) Uani 1 1 d . . . . .
C62 C 0.55893(17) 0.37676(17) 1.08904(12) 0.0342(5) Uani 1 1 d . . . . .
H62 H 0.5571 0.3932 1.1428 0.041 Uiso 1 1 calc R . . . .
C17 C 1.08681(16) 0.53207(18) 0.85798(12) 0.0317(5) Uani 1 1 d . . . . .
H17 H 1.1482 0.5357 0.8373 0.038 Uiso 1 1 calc R . . . .
C4 C 0.98854(15) 0.38806(19) 0.73351(13) 0.0349(5) Uani 1 1 d . . . . .
C27 C 0.55336(16) 0.39671(18) 0.56436(12) 0.0324(5) Uani 1 1 d . . . . .
C42 C 0.61702(18) 0.70876(17) 0.77275(14) 0.0373(5) Uani 1 1 d . . . . .
H42 H 0.6110 0.7744 0.7791 0.045 Uiso 1 1 calc R . . . .
C45 C 0.41969(18) -0.08359(18) 0.82345(14) 0.0397(5) Uani 1 1 d . . . . .
C26 C 0.50993(16) 0.42855(17) 0.63079(11) 0.0282(4) Uani 1 1 d . . . . .
C3 C 0.99920(17) 0.4300(2) 0.67327(13) 0.0428(6) Uani 1 1 d . . . . .
C48 C 0.48747(16) 0.13265(16) 0.91091(12) 0.0285(4) Uani 1 1 d . . . . .
C49 C 0.39016(17) 0.08032(17) 0.86597(13) 0.0336(5) Uani 1 1 d . . . . .
C23 C 0.3923(2) 0.2496(2) 0.50459(13) 0.0417(6) Uani 1 1 d . . . . .
C28 C 0.49285(19) 0.3079(2) 0.50271(13) 0.0396(5) Uani 1 1 d . . . . .
H28 H 0.5218 0.2865 0.4576 0.047 Uiso 1 1 calc R . . . .
C54 C 0.66001(16) 0.12947(17) 0.95084(13) 0.0340(5) Uani 1 1 d . . . . .
H54 H 0.6662 0.1969 0.9915 0.041 Uiso 1 1 calc R . . . .
C50 C 0.35859(17) -0.02713(18) 0.82310(13) 0.0369(5) Uani 1 1 d . . . . .
H50 H 0.2930 -0.0625 0.7927 0.044 Uiso 1 1 calc R . . . .
C25 C 0.40850(17) 0.37031(17) 0.63370(12) 0.0313(5) Uani 1 1 d . . . . .
C46 C 0.51556(18) -0.03056(18) 0.86589(14) 0.0391(5) Uani 1 1 d . . . . .
H46 H 0.5590 -0.0681 0.8656 0.047 Uiso 1 1 calc R . . . .
C5 C 0.97111(17) 0.2814(2) 0.71826(14) 0.0420(6) Uani 1 1 d . . . . .
C13 C 0.96424(19) 0.23736(19) 0.78309(15) 0.0436(6) Uani 1 1 d . . . . .
H13 H 0.9292 0.2736 0.8219 0.052 Uiso 1 1 calc R . . . .
C24 C 0.35183(18) 0.28254(18) 0.57084(13) 0.0369(5) Uani 1 1 d . . . . .
H24 H 0.2829 0.2436 0.5733 0.044 Uiso 1 1 calc R . . . .
C32 C 0.35864(18) 0.39995(19) 0.70451(13) 0.0406(6) Uani 1 1 d . . . . .
H32 H 0.4103 0.4653 0.7430 0.049 Uiso 1 1 calc R . . . .
C35 C 0.66239(18) 0.4589(2) 0.55793(14) 0.0419(6) Uani 1 1 d . . . . .
H35 H 0.6992 0.5041 0.6111 0.050 Uiso 1 1 calc R . . . .
C57 C 0.32030(18) 0.13914(19) 0.86505(15) 0.0417(6) Uani 1 1 d . . . . .
H57 H 0.3638 0.2126 0.8687 0.050 Uiso 1 1 calc R . . . .
C10 C 1.01426(18) 0.5443(2) 0.68894(14) 0.0456(6) Uani 1 1 d . . . . .
H10 H 1.0563 0.5858 0.7409 0.055 Uiso 1 1 calc R . . . .
C53 C 0.2871(2) -0.26354(19) 0.80238(16) 0.0501(6) Uani 1 1 d . . . . .
H53A H 0.2995 -0.2524 0.8574 0.075 Uiso 1 1 calc GR . . . .
H53B H 0.2666 -0.3387 0.7726 0.075 Uiso 1 1 calc GR . . . .
H53C H 0.2325 -0.2399 0.7927 0.075 Uiso 1 1 calc GR . . . .
C55 C 0.73274(19) 0.1569(2) 0.89492(17) 0.0536(7) Uani 1 1 d . . . . .
H55A H 0.7247 0.0924 0.8524 0.080 Uiso 1 1 calc GR . . . .
H55B H 0.8031 0.1899 0.9217 0.080 Uiso 1 1 calc GR . . . .
H55C H 0.7174 0.2060 0.8746 0.080 Uiso 1 1 calc GR . . . .
C2 C 0.9909(2) 0.3638(3) 0.59887(15) 0.0588(8) Uani 1 1 d . . . . .
H2 H 0.9975 0.3917 0.5582 0.071 Uiso 1 1 calc R . . . .
C51 C 0.3827(2) -0.2017(2) 0.77851(17) 0.0511(7) Uani 1 1 d . . . . .
H51 H 0.4371 -0.2266 0.7898 0.061 Uiso 1 1 calc R . . . .
C56 C 0.6906(2) 0.0638(2) 0.99002(17) 0.0511(6) Uani 1 1 d . . . . .
H56A H 0.6388 0.0396 1.0213 0.077 Uiso 1 1 calc GR . . . .
H56B H 0.7565 0.1068 1.0232 0.077 Uiso 1 1 calc GR . . . .
H56C H 0.6961 0.0026 0.9509 0.077 Uiso 1 1 calc GR . . . .
C1 C 0.9733(2) 0.2581(3) 0.58196(16) 0.0678(9) Uani 1 1 d . . . . .
C67 C 0.6818(2) 0.2167(2) 0.65675(14) 0.0516(7) Uani 1 1 d . . . . .
H67A H 0.7307 0.1812 0.6547 0.062 Uiso 1 1 calc R . . . .
H67B H 0.7181 0.2876 0.6537 0.062 Uiso 1 1 calc R . . . .
C59 C 0.2643(2) 0.1462(2) 0.93479(17) 0.0555(7) Uani 1 1 d . . . . .
H59A H 0.2227 0.0750 0.9335 0.083 Uiso 1 1 calc GR . . . .
H59B H 0.2201 0.1852 0.9336 0.083 Uiso 1 1 calc GR . . . .
H59C H 0.3140 0.1831 0.9821 0.083 Uiso 1 1 calc GR . . . .
C6 C 0.9645(2) 0.2181(2) 0.64199(16) 0.0565(7) Uani 1 1 d . . . . .
H6 H 0.9538 0.1459 0.6310 0.068 Uiso 1 1 calc R . . . .
C11 C 0.9118(2) 0.5572(3) 0.69313(17) 0.0554(7) Uani 1 1 d . . . . .
H11A H 0.8700 0.5212 0.6421 0.083 Uiso 1 1 calc GR . . . .
H11B H 0.9233 0.6323 0.7100 0.083 Uiso 1 1 calc GR . . . .
H11C H 0.8764 0.5262 0.7299 0.083 Uiso 1 1 calc GR . . . .
C69 C 0.5184(2) 0.0819(2) 0.62669(17) 0.0647(8) Uani 1 1 d . . . . .
H69A H 0.4480 0.0595 0.6009 0.078 Uiso 1 1 calc R . . . .
H69B H 0.5335 0.0184 0.6223 0.078 Uiso 1 1 calc R . . . .
C15 C 1.0709(2) 0.2636(2) 0.82331(18) 0.0568(7) Uani 1 1 d . . . . .
H15A H 1.1082 0.2307 0.7865 0.085 Uiso 1 1 calc GR . . . .
H15B H 1.0648 0.2366 0.8662 0.085 Uiso 1 1 calc GR . . . .
H15C H 1.1079 0.3402 0.8430 0.085 Uiso 1 1 calc GR . . . .
C70 C 0.5317(2) 0.1483(2) 0.70783(17) 0.0645(9) Uani 1 1 d . . . . .
H70A H 0.4834 0.1850 0.7150 0.077 Uiso 1 1 calc R . . . .
H70B H 0.5193 0.1047 0.7414 0.077 Uiso 1 1 calc R . . . .
C29 C 0.3255(3) 0.1522(2) 0.43759(16) 0.0638(8) Uani 1 1 d . . . . .
H29 H 0.2627 0.1668 0.4300 0.077 Uiso 0.580(7) 1 calc R . P A 1
H29A H 0.3747 0.1382 0.4019 0.077 Uiso 0.420(7) 1 calc R . P A 2
C58 C 0.2435(2) 0.0895(2) 0.79064(18) 0.0561(7) Uani 1 1 d . . . . .
H58A H 0.2801 0.0830 0.7461 0.084 Uiso 1 1 calc GR . . . .
H58B H 0.2051 0.1343 0.7905 0.084 Uiso 1 1 calc GR . . . .
H58C H 0.1962 0.0194 0.7878 0.084 Uiso 1 1 calc GR . . . .
C33 C 0.2679(3) 0.4254(3) 0.6878(2) 0.0684(9) Uani 1 1 d . . . . .
H33A H 0.2885 0.4812 0.6651 0.103 Uiso 1 1 calc GR . . . .
H33B H 0.2417 0.4494 0.7358 0.103 Uiso 1 1 calc GR . . . .
H33C H 0.2146 0.3622 0.6516 0.103 Uiso 1 1 calc GR . . . .
C68 C 0.5942(3) 0.1530(3) 0.59288(17) 0.0689(9) Uani 1 1 d . . . . .
H68A H 0.6154 0.1115 0.5473 0.083 Uiso 1 1 calc R . . . .
H68B H 0.5655 0.1988 0.5776 0.083 Uiso 1 1 calc R . . . .
C34 C 0.3310(3) 0.3142(3) 0.74091(16) 0.0622(8) Uani 1 1 d . . . . .
H34A H 0.2813 0.2484 0.7043 0.093 Uiso 1 1 calc GR . . . .
H34B H 0.3014 0.3360 0.7876 0.093 Uiso 1 1 calc GR . . . .
H34C H 0.3926 0.3030 0.7542 0.093 Uiso 1 1 calc GR . . . .
C8 C 0.8595(3) 0.1648(3) 0.45410(17) 0.0759(10) Uani 1 1 d . . . . .
H8A H 0.8046 0.1246 0.4765 0.114 Uiso 1 1 calc GR . . . .
H8B H 0.8554 0.1234 0.4000 0.114 Uiso 1 1 calc GR . . . .
H8C H 0.8525 0.2312 0.4574 0.114 Uiso 1 1 calc GR . . . .
C30 C 0.2872(3) 0.0572(2) 0.45984(19) 0.0715(9) Uani 1 1 d . . . . .
H30A H 0.3450 0.0447 0.4792 0.107 Uiso 1 1 calc GR . . . .
H30B H 0.2466 -0.0038 0.4149 0.107 Uiso 1 1 calc GR . . . .
H30C H 0.2446 0.0677 0.5002 0.107 Uiso 1 1 calc GR . . . .
C14 C 0.9028(3) 0.1188(2) 0.7591(2) 0.0683(9) Uani 1 1 d . . . . .
H14A H 0.8356 0.1018 0.7316 0.102 Uiso 1 1 calc GR . . . .
H14B H 0.8945 0.0982 0.8051 0.102 Uiso 1 1 calc GR . . . .
H14C H 0.9391 0.0804 0.7253 0.102 Uiso 1 1 calc GR . . . .
C12 C 1.0709(2) 0.5924(3) 0.63179(18) 0.0690(9) Uani 1 1 d . . . . .
H12A H 1.1346 0.5799 0.6273 0.103 Uiso 1 1 calc GR . . . .
H12B H 1.0864 0.6684 0.6502 0.103 Uiso 1 1 calc GR . . . .
H12C H 1.0279 0.5595 0.5813 0.103 Uiso 1 1 calc GR . . . .
C52 C 0.3682(3) -0.2219(3) 0.69320(19) 0.0842(12) Uani 1 1 d . . . . .
H52A H 0.3198 -0.1923 0.6811 0.126 Uiso 1 1 calc GR . . . .
H52B H 0.3416 -0.2981 0.6652 0.126 Uiso 1 1 calc GR . . . .
H52C H 0.4339 -0.1885 0.6778 0.126 Uiso 1 1 calc GR . . . .
C36 C 0.7202(2) 0.3894(3) 0.52059(18) 0.0747(10) Uani 1 1 d . . . . .
H36A H 0.7208 0.3438 0.5503 0.112 Uiso 1 1 calc GR . . . .
H36B H 0.7905 0.4340 0.5197 0.112 Uiso 1 1 calc GR . . . .
H36C H 0.6865 0.3457 0.4678 0.112 Uiso 1 1 calc GR . . . .
C37 C 0.6627(3) 0.5303(5) 0.5136(3) 0.131(2) Uani 1 1 d . . . . .
H37A H 0.6164 0.4891 0.4647 0.196 Uiso 1 1 calc GR . . . .
H37B H 0.7320 0.5628 0.5032 0.196 Uiso 1 1 calc GR . . . .
H37C H 0.6400 0.5854 0.5438 0.196 Uiso 1 1 calc GR . . . .
C7 C 0.9617(4) 0.1883(4) 0.4979(2) 0.1096(17) Uani 1 1 d . . . . .
H7A H 1.0112 0.2367 0.4755 0.132 Uiso 0.5 1 calc R . P B 1
H7B H 0.9440 0.1195 0.5067 0.132 Uiso 0.5 1 calc R . P C 2
C31A C 0.3556(4) 0.1334(4) 0.3643(2) 0.0521(15) Uani 0.580(7) 1 d . . P A 1
H31A H 0.3713 0.1968 0.3502 0.078 Uiso 0.580(7) 1 calc GR . P A 1
H31B H 0.3001 0.0746 0.3265 0.078 Uiso 0.580(7) 1 calc GR . P A 1
H31C H 0.4163 0.1158 0.3651 0.078 Uiso 0.580(7) 1 calc GR . P A 1
C31 C 0.2567(7) 0.1863(6) 0.3922(4) 0.079(3) Uani 0.420(7) 1 d . . P A 2
H31D H 0.2055 0.2021 0.4232 0.118 Uiso 0.420(7) 1 calc GR . P A 2
H31E H 0.2224 0.1289 0.3436 0.118 Uiso 0.420(7) 1 calc GR . P A 2
H31F H 0.2991 0.2494 0.3814 0.118 Uiso 0.420(7) 1 calc GR . P A 2
C9A C 0.9980(6) 0.1041(6) 0.4864(4) 0.0681(19) Uani 0.5 1 d . U P D 1
H9AA H 1.0642 0.1307 0.5188 0.102 Uiso 0.5 1 calc GR . P D 1
H9AB H 1.0056 0.0769 0.4322 0.102 Uiso 0.5 1 calc GR . P D 1
H9AC H 0.9490 0.0474 0.5005 0.102 Uiso 0.5 1 calc GR . P D 1
C9B C 1.0357(8) 0.1871(13) 0.4669(5) 0.172(7) Uani 0.5 1 d . U P D 2
H9BA H 1.0748 0.2576 0.4657 0.257 Uiso 0.5 1 calc GR . P D 2
H9BB H 1.0136 0.1367 0.4142 0.257 Uiso 0.5 1 calc GR . P D 2
H9BC H 1.0785 0.1660 0.4957 0.257 Uiso 0.5 1 calc GR . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O1 1.8783(14) . ?
Cr1 O3 1.8902(14) . ?
Cr1 O2 1.8562(14) . ?
Cr1 O5 2.0410(14) . ?
Cr1 N1 2.0672(16) . ?
O1 C21 1.342(2) . ?
O3 C65 1.339(2) . ?
O2 C39 1.338(2) . ?
O5 C67 1.447(3) . ?
O5 C70 1.452(3) . ?
N1 C44 1.492(2) . ?
N1 C22 1.503(2) . ?
N1 C66 1.500(2) . ?
C64 C65 1.401(3) . ?
C64 C63 1.390(3) . ?
C64 C66 1.496(3) . ?
C65 C60 1.409(3) . ?
C39 C40 1.402(3) . ?
C39 C38 1.410(3) . ?
C40 C44 1.501(3) . ?
C40 C41 1.391(3) . ?
C20 C21 1.398(3) . ?
C20 C19 1.390(3) . ?
C20 C22 1.504(3) . ?
C38 C43 1.386(3) . ?
C38 C26 1.496(3) . ?
C21 C16 1.406(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C16 C17 1.397(3) . ?
C16 C4 1.497(3) . ?
C60 C61 1.393(3) . ?
C60 C48 1.497(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.386(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C43 H43 0.9500 . ?
C43 C42 1.385(3) . ?
C63 H63 0.9500 . ?
C63 C62 1.383(3) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C61 H61 0.9500 . ?
C61 C62 1.383(3) . ?
C18 H18 0.9500 . ?
C18 C17 1.377(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.380(3) . ?
C47 C48 1.403(3) . ?
C47 C54 1.518(3) . ?
C47 C46 1.392(3) . ?
C62 H62 0.9500 . ?
C17 H17 0.9500 . ?
C4 C3 1.411(3) . ?
C4 C5 1.402(4) . ?
C27 C26 1.407(3) . ?
C27 C28 1.394(3) . ?
C27 C35 1.518(3) . ?
C42 H42 0.9500 . ?
C45 C50 1.382(4) . ?
C45 C46 1.374(3) . ?
C45 C51 1.527(3) . ?
C26 C25 1.398(3) . ?
C3 C10 1.514(4) . ?
C3 C2 1.383(4) . ?
C48 C49 1.408(3) . ?
C49 C50 1.399(3) . ?
C49 C57 1.515(3) . ?
C23 C28 1.384(4) . ?
C23 C24 1.384(3) . ?
C23 C29 1.524(3) . ?
C28 H28 0.9500 . ?
C54 H54 1.0000 . ?
C54 C55 1.518(3) . ?
C54 C56 1.520(3) . ?
C50 H50 0.9500 . ?
C25 C24 1.385(3) . ?
C25 C32 1.517(3) . ?
C46 H46 0.9500 . ?
C5 C13 1.511(4) . ?
C5 C6 1.400(3) . ?
C13 H13 1.0000 . ?
C13 C15 1.532(4) . ?
C13 C14 1.529(4) . ?
C24 H24 0.9500 . ?
C32 H32 1.0000 . ?
C32 C33 1.505(4) . ?
C32 C34 1.525(4) . ?
C35 H35 1.0000 . ?
C35 C36 1.525(4) . ?
C35 C37 1.500(4) . ?
C57 H57 1.0000 . ?
C57 C59 1.525(4) . ?
C57 C58 1.534(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.527(4) . ?
C10 C12 1.532(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C53 C51 1.499(4) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C2 H2 0.9500 . ?
C2 C1 1.383(5) . ?
C51 H51 1.0000 . ?
C51 C52 1.507(4) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C1 C6 1.390(5) . ?
C1 C7 1.532(4) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.493(4) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C6 H6 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.472(4) . ?
C69 C68 1.501(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C29 H29 1.0000 . ?
C29 H29A 1.0000 . ?
C29 C30 1.476(5) . ?
C29 C31A 1.403(5) . ?
C29 C31 1.565(9) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C7 1.514(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C7 C9A 1.436(9) . ?
C7 C9B 1.209(10) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C31 H31D 0.9800 . ?
C31 H31E 0.9800 . ?
C31 H31F 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cr1 O3 140.86(7) . . ?
O1 Cr1 O5 87.13(6) . . ?
O1 Cr1 N1 91.06(6) . . ?
O3 Cr1 O5 86.27(6) . . ?
O3 Cr1 N1 93.33(6) . . ?
O2 Cr1 O1 108.43(7) . . ?
O2 Cr1 O3 110.08(7) . . ?
O2 Cr1 O5 89.85(6) . . ?
O2 Cr1 N1 93.46(6) . . ?
O5 Cr1 N1 176.59(6) . . ?
C21 O1 Cr1 132.14(13) . . ?
C65 O3 Cr1 124.05(12) . . ?
C39 O2 Cr1 130.83(12) . . ?
C67 O5 Cr1 118.97(14) . . ?
C67 O5 C70 109.24(19) . . ?
C70 O5 Cr1 122.08(15) . . ?
C44 N1 Cr1 111.02(11) . . ?
C44 N1 C22 109.24(15) . . ?
C44 N1 C66 108.84(14) . . ?
C22 N1 Cr1 107.86(11) . . ?
C66 N1 Cr1 110.36(11) . . ?
C66 N1 C22 109.49(14) . . ?
C65 C64 C66 118.56(17) . . ?
C63 C64 C65 119.75(19) . . ?
C63 C64 C66 121.69(18) . . ?
O3 C65 C64 120.31(18) . . ?
O3 C65 C60 119.73(18) . . ?
C64 C65 C60 119.95(18) . . ?
O2 C39 C40 121.67(17) . . ?
O2 C39 C38 118.32(18) . . ?
C40 C39 C38 120.01(18) . . ?
C39 C40 C44 120.62(17) . . ?
C41 C40 C39 119.31(18) . . ?
C41 C40 C44 119.85(18) . . ?
C21 C20 C22 119.98(18) . . ?
C19 C20 C21 119.54(19) . . ?
C19 C20 C22 120.46(18) . . ?
C39 C38 C26 119.81(18) . . ?
C43 C38 C39 118.70(19) . . ?
C43 C38 C26 121.45(18) . . ?
O1 C21 C20 120.93(18) . . ?
O1 C21 C16 118.90(18) . . ?
C20 C21 C16 120.17(18) . . ?
N1 C44 C40 115.04(16) . . ?
N1 C44 H44A 108.5 . . ?
N1 C44 H44B 108.5 . . ?
C40 C44 H44A 108.5 . . ?
C40 C44 H44B 108.5 . . ?
H44A C44 H44B 107.5 . . ?
C21 C16 C4 120.06(18) . . ?
C17 C16 C21 118.48(19) . . ?
C17 C16 C4 121.42(19) . . ?
C65 C60 C48 121.15(18) . . ?
C61 C60 C65 118.47(19) . . ?
C61 C60 C48 120.35(18) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 C20 120.8(2) . . ?
C18 C19 H19 119.6 . . ?
N1 C22 C20 113.84(15) . . ?
N1 C22 H22A 108.8 . . ?
N1 C22 H22B 108.8 . . ?
C20 C22 H22A 108.8 . . ?
C20 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C38 C43 H43 119.2 . . ?
C42 C43 C38 121.6(2) . . ?
C42 C43 H43 119.2 . . ?
C64 C63 H63 119.7 . . ?
C62 C63 C64 120.69(19) . . ?
C62 C63 H63 119.7 . . ?
N1 C66 H66A 109.0 . . ?
N1 C66 H66B 109.0 . . ?
C64 C66 N1 113.02(15) . . ?
C64 C66 H66A 109.0 . . ?
C64 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
C60 C61 H61 119.2 . . ?
C62 C61 C60 121.7(2) . . ?
C62 C61 H61 119.2 . . ?
C19 C18 H18 120.3 . . ?
C17 C18 C19 119.43(19) . . ?
C17 C18 H18 120.3 . . ?
C40 C41 H41 119.5 . . ?
C42 C41 C40 121.0(2) . . ?
C42 C41 H41 119.5 . . ?
C48 C47 C54 122.04(19) . . ?
C46 C47 C48 119.7(2) . . ?
C46 C47 C54 118.2(2) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 C63 119.5(2) . . ?
C61 C62 H62 120.3 . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(2) . . ?
C18 C17 H17 119.2 . . ?
C3 C4 C16 119.7(2) . . ?
C5 C4 C16 119.8(2) . . ?
C5 C4 C3 120.5(2) . . ?
C26 C27 C35 121.4(2) . . ?
C28 C27 C26 118.5(2) . . ?
C28 C27 C35 120.0(2) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 C43 119.4(2) . . ?
C41 C42 H42 120.3 . . ?
C50 C45 C51 121.6(2) . . ?
C46 C45 C50 118.1(2) . . ?
C46 C45 C51 120.3(2) . . ?
C27 C26 C38 120.80(19) . . ?
C25 C26 C38 119.61(18) . . ?
C25 C26 C27 119.6(2) . . ?
C4 C3 C10 120.8(2) . . ?
C2 C3 C4 118.8(3) . . ?
C2 C3 C10 120.3(2) . . ?
C47 C48 C60 119.44(19) . . ?
C47 C48 C49 119.04(19) . . ?
C49 C48 C60 121.51(19) . . ?
C48 C49 C57 120.5(2) . . ?
C50 C49 C48 118.9(2) . . ?
C50 C49 C57 120.6(2) . . ?
C28 C23 C24 117.6(2) . . ?
C28 C23 C29 123.0(2) . . ?
C24 C23 C29 119.4(2) . . ?
C27 C28 H28 118.7 . . ?
C23 C28 C27 122.6(2) . . ?
C23 C28 H28 118.7 . . ?
C47 C54 H54 107.8 . . ?
C47 C54 C55 109.71(19) . . ?
C47 C54 C56 113.43(19) . . ?
C55 C54 H54 107.8 . . ?
C55 C54 C56 110.2(2) . . ?
C56 C54 H54 107.8 . . ?
C45 C50 C49 122.2(2) . . ?
C45 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
C26 C25 C32 121.71(19) . . ?
C24 C25 C26 119.5(2) . . ?
C24 C25 C32 118.8(2) . . ?
C47 C46 H46 119.0 . . ?
C45 C46 C47 122.0(2) . . ?
C45 C46 H46 119.0 . . ?
C4 C5 C13 120.6(2) . . ?
C6 C5 C4 118.2(3) . . ?
C6 C5 C13 121.1(3) . . ?
C5 C13 H13 107.2 . . ?
C5 C13 C15 110.7(2) . . ?
C5 C13 C14 114.5(2) . . ?
C15 C13 H13 107.2 . . ?
C14 C13 H13 107.2 . . ?
C14 C13 C15 109.6(2) . . ?
C23 C24 C25 122.2(2) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C25 C32 H32 107.3 . . ?
C25 C32 C34 110.7(2) . . ?
C33 C32 C25 112.4(2) . . ?
C33 C32 H32 107.3 . . ?
C33 C32 C34 111.6(2) . . ?
C34 C32 H32 107.3 . . ?
C27 C35 H35 108.0 . . ?
C27 C35 C36 113.4(2) . . ?
C36 C35 H35 108.0 . . ?
C37 C35 C27 109.6(2) . . ?
C37 C35 H35 108.0 . . ?
C37 C35 C36 109.8(3) . . ?
C49 C57 H57 107.8 . . ?
C49 C57 C59 110.6(2) . . ?
C49 C57 C58 112.6(2) . . ?
C59 C57 H57 107.8 . . ?
C59 C57 C58 110.1(2) . . ?
C58 C57 H57 107.8 . . ?
C3 C10 H10 107.1 . . ?
C3 C10 C11 110.2(2) . . ?
C3 C10 C12 114.7(2) . . ?
C11 C10 H10 107.1 . . ?
C11 C10 C12 110.2(2) . . ?
C12 C10 H10 107.1 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C3 C2 H2 119.0 . . ?
C3 C2 C1 122.0(3) . . ?
C1 C2 H2 119.0 . . ?
C45 C51 H51 107.7 . . ?
C53 C51 C45 112.2(2) . . ?
C53 C51 H51 107.7 . . ?
C53 C51 C52 111.0(2) . . ?
C52 C51 C45 110.4(2) . . ?
C52 C51 H51 107.7 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C2 C1 C6 118.6(3) . . ?
C2 C1 C7 119.3(4) . . ?
C6 C1 C7 122.1(4) . . ?
O5 C67 H67A 110.8 . . ?
O5 C67 H67B 110.8 . . ?
O5 C67 C68 104.9(2) . . ?
H67A C67 H67B 108.9 . . ?
C68 C67 H67A 110.8 . . ?
C68 C67 H67B 110.8 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C5 C6 H6 119.1 . . ?
C1 C6 C5 121.8(3) . . ?
C1 C6 H6 119.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H69A C69 H69B 109.0 . . ?
C70 C69 H69A 111.1 . . ?
C70 C69 H69B 111.1 . . ?
C70 C69 C68 103.4(2) . . ?
C68 C69 H69A 111.1 . . ?
C68 C69 H69B 111.1 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O5 C70 C69 106.4(2) . . ?
O5 C70 H70A 110.4 . . ?
O5 C70 H70B 110.4 . . ?
C69 C70 H70A 110.4 . . ?
C69 C70 H70B 110.4 . . ?
H70A C70 H70B 108.6 . . ?
C23 C29 H29 102.9 . . ?
C23 C29 H29A 103.6 . . ?
C23 C29 C31 107.7(4) . . ?
C30 C29 C23 112.1(2) . . ?
C30 C29 H29 102.9 . . ?
C30 C29 H29A 103.6 . . ?
C30 C29 C31 123.8(4) . . ?
C31A C29 C23 119.7(3) . . ?
C31A C29 H29 102.9 . . ?
C31A C29 C30 113.6(3) . . ?
C31 C29 H29A 103.6 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C67 C68 C69 103.7(2) . . ?
C67 C68 H68A 111.0 . . ?
C67 C68 H68B 111.0 . . ?
C69 C68 H68A 111.0 . . ?
C69 C68 H68B 111.0 . . ?
H68A C68 H68B 109.0 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C1 C7 H7A 103.1 . . ?
C1 C7 H7B 97.6 . . ?
C8 C7 C1 111.0(3) . . ?
C8 C7 H7A 103.1 . . ?
C8 C7 H7B 97.6 . . ?
C9A C7 C1 115.3(4) . . ?
C9A C7 C8 118.7(5) . . ?
C9A C7 H7A 103.1 . . ?
C9B C7 C1 121.0(6) . . ?
C9B C7 C8 122.9(7) . . ?
C9B C7 H7B 97.6 . . ?
C29 C31A H31A 109.5 . . ?
C29 C31A H31B 109.5 . . ?
C29 C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C29 C31 H31D 109.5 . . ?
C29 C31 H31E 109.5 . . ?
C29 C31 H31F 109.5 . . ?
H31D C31 H31E 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7 C9B H9BA 109.5 . . ?
C7 C9B H9BB 109.5 . . ?
C7 C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 75.8 electrons were 
found in a volume of 426.5 A^3 in one void. 
This is consistent with the presence of 
1.8 [n-pentane] per formula unit 
which account for 75.6 electrons.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 426.5 75.8 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c2c_1
_database_code_depnum_ccdc_archive 'CCDC 1894392'
loop_
_audit_author_name
_audit_author_address
'Dae Young Bae'
;Pohang University of Science and Technology
South Korea
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_c2c_1               
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 6.2 Ratio
RESPONSE: This alert results from the disorder on the isopropyl groups. 
It is unremarkable for the methyl carbon atoms of isopropyl groups to show moderate rotolibrations. 
This leads larger Ueq values for those carbon atoms than rigidly bound carbon atoms. 
This does not mean incorrect atomic identification even though the methyl carbon atoms on the isopropyl groups show high Ueq values.
;
# end Validation Reply Form

_audit_creation_date             2019-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C70 H92 N O4 V'
_chemical_formula_sum            'C70 H92 N O4 V'
_chemical_formula_weight         1062.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   37.206(7)
_cell_length_b                   14.294(3)
_cell_length_c                   24.650(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.33(3)
_cell_angle_gamma                90
_cell_volume                     13053(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10736
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.527
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light navy'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    navy
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19755
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.527
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7000
_diffrn_source                   'PLSII 2D bending magnet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9784
_reflns_number_total             10736
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10736
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0862
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1599P)²+30.3613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2498
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
3. Others
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C57(H57), C32(H32), C10(H10), C35(H35), C54(H54), C13(H13), C51(H51),
 C29(H29), C7(H7A), C7(H7B)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C66(H66A,H66B), C44(H44A,H44B), C70(H70A,H70B), C69(H69A,
 H69B), C68(H68A,H68B), C67(H67A,H67B)
4.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C63(H63), C40(H40), C61(H61), C41(H41), C62(H62), C17(H17),
 C19(H19), C50(H50), C46(H46), C18(H18), C24(H24), C28(H28), C6(H6), C2(H2)
4.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C12(H12A,H12B,H12C), C37(H37A,H37B,
 H37C), C11(H11A,H11B,H11C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C34(H34A,
 H34B,H34C), C33(H33A,H33B,H33C), C55(H55A,H55B,H55C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C),
  C9(H9A,H9B,H9C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.40815(2) 0.26147(3) 0.45450(2) 0.02888(19) Uani 1 1 d . . . . .
O2 O 0.39299(5) 0.31670(13) 0.38768(8) 0.0320(5) Uani 1 1 d . . . . .
O3 O 0.41775(5) 0.33983(15) 0.51478(9) 0.0354(5) Uani 1 1 d . . . . .
O1 O 0.41059(5) 0.13090(14) 0.46077(8) 0.0330(5) Uani 1 1 d . . . . .
O4 O 0.35388(6) 0.25389(15) 0.47134(11) 0.0440(6) Uani 1 1 d . . . . .
N6 N 0.46349(7) 0.26745(15) 0.43685(10) 0.0296(5) Uani 1 1 d . . . . .
C43 C 0.41139(8) 0.35934(19) 0.34969(11) 0.0298(6) Uani 1 1 d . . . . .
C42 C 0.44753(8) 0.33619(19) 0.34366(11) 0.0306(6) Uani 1 1 d . . . . .
C21 C 0.43532(8) 0.0692(2) 0.44575(12) 0.0340(6) Uani 1 1 d . . . . .
C39 C 0.41228(8) 0.4720(2) 0.27706(12) 0.0348(6) Uani 1 1 d . . . . .
H39 H 0.400661 0.516810 0.254411 0.042 Uiso 1 1 calc R . . . .
C64 C 0.48094(8) 0.3728(2) 0.51625(13) 0.0339(6) Uani 1 1 d . . . . .
C65 C 0.44905(8) 0.3652(2) 0.54270(13) 0.0334(6) Uani 1 1 d . . . . .
C63 C 0.51317(8) 0.3960(2) 0.54716(14) 0.0403(7) Uani 1 1 d . . . . .
H63 H 0.534390 0.400178 0.530135 0.048 Uiso 1 1 calc R . . . .
C38 C 0.39354(8) 0.4283(2) 0.31653(12) 0.0313(6) Uani 1 1 d . . . . .
C26 C 0.35576(8) 0.4568(2) 0.32547(12) 0.0358(7) Uani 1 1 d . . . . .
C48 C 0.41557(8) 0.3724(2) 0.62616(12) 0.0337(6) Uani 1 1 d . . . . .
C49 C 0.38863(8) 0.4414(2) 0.62063(12) 0.0353(7) Uani 1 1 d . . . . .
C22 C 0.48414(8) 0.1893(2) 0.46568(13) 0.0351(7) Uani 1 1 d . . . . .
H22A H 0.481670 0.194157 0.504412 0.042 Uiso 1 1 calc R . . . .
H22B H 0.509524 0.196395 0.460514 0.042 Uiso 1 1 calc R . . . .
C40 C 0.44795(9) 0.4495(2) 0.27109(12) 0.0374(7) Uani 1 1 d . . . . .
H40 H 0.460091 0.479302 0.244651 0.045 Uiso 1 1 calc R . . . .
C61 C 0.48230(9) 0.4064(2) 0.62782(14) 0.0395(7) Uani 1 1 d . . . . .
H61 H 0.482893 0.417952 0.665019 0.047 Uiso 1 1 calc R . . . .
C20 C 0.47190(8) 0.0941(2) 0.44637(12) 0.0345(6) Uani 1 1 d . . . . .
C25 C 0.35043(9) 0.5394(2) 0.35457(13) 0.0411(7) Uani 1 1 d . . . . .
C60 C 0.44951(8) 0.3830(2) 0.59860(13) 0.0343(6) Uani 1 1 d . . . . .
C41 C 0.46550(8) 0.3826(2) 0.30458(12) 0.0343(6) Uani 1 1 d . . . . .
H41 H 0.489558 0.368550 0.300867 0.041 Uiso 1 1 calc R . . . .
C47 C 0.41008(9) 0.2913(2) 0.65537(15) 0.0446(8) Uani 1 1 d . . . . .
C16 C 0.42376(9) -0.0207(2) 0.42910(14) 0.0396(7) Uani 1 1 d . . . . .
C66 C 0.47973(8) 0.3589(2) 0.45626(13) 0.0355(7) Uani 1 1 d . . . . .
H66A H 0.504104 0.362773 0.445488 0.043 Uiso 1 1 calc R . . . .
H66B H 0.465874 0.409400 0.438242 0.043 Uiso 1 1 calc R . . . .
C62 C 0.51408(9) 0.4126(2) 0.60231(14) 0.0423(8) Uani 1 1 d . . . . .
H62 H 0.535710 0.427850 0.622320 0.051 Uiso 1 1 calc R . . . .
C17 C 0.44942(10) -0.0845(2) 0.41424(15) 0.0449(8) Uani 1 1 d . . . . .
H17 H 0.442141 -0.144610 0.403910 0.054 Uiso 1 1 calc R . . . .
C19 C 0.49661(9) 0.0282(2) 0.43072(13) 0.0386(7) Uani 1 1 d . . . . .
H19 H 0.520855 0.044300 0.431239 0.046 Uiso 1 1 calc R . . . .
C50 C 0.35665(9) 0.4264(2) 0.64467(13) 0.0410(7) Uani 1 1 d . . . . .
H50 H 0.338878 0.472382 0.641405 0.049 Uiso 1 1 calc R . . . .
C44 C 0.46600(9) 0.2589(2) 0.37702(13) 0.0342(7) Uani 1 1 d . . . . .
H44A H 0.455456 0.199597 0.364738 0.041 Uiso 1 1 calc R . . . .
H44B H 0.491275 0.257710 0.370332 0.041 Uiso 1 1 calc R . . . .
C57 C 0.39446(9) 0.5308(2) 0.58887(13) 0.0411(7) Uani 1 1 d . . . . .
H57 H 0.405752 0.513219 0.555980 0.049 Uiso 1 1 calc R . . . .
C46 C 0.37748(9) 0.2799(3) 0.67869(16) 0.0491(9) Uani 1 1 d . . . . .
H46 H 0.374018 0.225914 0.698598 0.059 Uiso 1 1 calc R . . . .
C59 C 0.42039(10) 0.5976(2) 0.62186(16) 0.0496(8) Uani 1 1 d . . . . .
H59A H 0.409382 0.619182 0.653268 0.074 Uiso 1 1 calc GR . . . .
H59B H 0.425603 0.650048 0.599594 0.074 Uiso 1 1 calc GR . . . .
H59C H 0.442389 0.565167 0.633338 0.074 Uiso 1 1 calc GR . . . .
C18 C 0.48559(9) -0.0604(2) 0.41449(15) 0.0439(8) Uani 1 1 d . . . . .
H18 H 0.502227 -0.103649 0.403811 0.053 Uiso 1 1 calc R . . . .
C4 C 0.38452(9) -0.0463(2) 0.42550(16) 0.0473(9) Uani 1 1 d . . . . .
C45 C 0.35044(9) 0.3454(3) 0.67330(14) 0.0478(8) Uani 1 1 d . . . . .
C5 C 0.36793(10) -0.0719(2) 0.47132(19) 0.0544(10) Uani 1 1 d . . . . .
C58 C 0.35923(10) 0.5822(3) 0.57066(15) 0.0503(8) Uani 1 1 d . . . . .
H58A H 0.343191 0.540671 0.549582 0.076 Uiso 1 1 calc GR . . . .
H58B H 0.364381 0.635393 0.548871 0.076 Uiso 1 1 calc GR . . . .
H58C H 0.348049 0.602858 0.602137 0.076 Uiso 1 1 calc GR . . . .
C24 C 0.31546(11) 0.5652(3) 0.36318(18) 0.0594(10) Uani 1 1 d . . . . .
H24 H 0.311910 0.620199 0.382116 0.071 Uiso 1 1 calc R . . . .
C32 C 0.38133(10) 0.6010(3) 0.37585(15) 0.0506(9) Uani 1 1 d . . . . .
H32 H 0.403579 0.566524 0.371084 0.061 Uiso 1 1 calc R . . . .
C27 C 0.32579(9) 0.4008(2) 0.30621(15) 0.0448(8) Uani 1 1 d . . . . .
C10 C 0.38916(10) -0.0753(2) 0.52695(18) 0.0541(9) Uani 1 1 d . . . . .
H10 H 0.407321 -0.025482 0.528047 0.065 Uiso 1 1 calc R . . . .
C35 C 0.33121(10) 0.3132(2) 0.27307(17) 0.0510(9) Uani 1 1 d . . . . .
H35 H 0.353919 0.284147 0.287701 0.061 Uiso 1 1 calc R . . . .
C3 C 0.36488(11) -0.0441(3) 0.3733(2) 0.0597(11) Uani 1 1 d . . . . .
C28 C 0.29148(10) 0.4303(3) 0.31676(19) 0.0609(10) Uani 1 1 d . . . . .
H28 H 0.271711 0.393662 0.304587 0.073 Uiso 1 1 calc R . . . .
C12 C 0.40933(12) -0.1688(3) 0.5353(2) 0.0654(11) Uani 1 1 d . . . . .
H12A H 0.392190 -0.219082 0.534327 0.098 Uiso 1 1 calc GR . . . .
H12B H 0.423448 -0.168353 0.569892 0.098 Uiso 1 1 calc GR . . . .
H12C H 0.424937 -0.177256 0.506752 0.098 Uiso 1 1 calc GR . . . .
C54 C 0.43782(11) 0.2130(3) 0.6615(2) 0.0669(12) Uani 1 1 d . . . . .
H54 H 0.458891 0.232828 0.643324 0.080 Uiso 1 1 calc R . . . .
C23 C 0.28561(12) 0.5122(4) 0.3447(2) 0.0733(13) Uani 1 1 d . . . . .
C6 C 0.33155(12) -0.0975(3) 0.4653(2) 0.0780(15) Uani 1 1 d . . . . .
H6 H 0.320263 -0.116528 0.495566 0.094 Uiso 1 1 calc R . . . .
C37 C 0.30114(14) 0.2404(3) 0.2755(2) 0.0761(14) Uani 1 1 d . . . . .
H37A H 0.297544 0.227614 0.312860 0.114 Uiso 1 1 calc GR . . . .
H37B H 0.307883 0.183720 0.258136 0.114 Uiso 1 1 calc GR . . . .
H37C H 0.279163 0.264110 0.257053 0.114 Uiso 1 1 calc GR . . . .
C11 C 0.36606(13) -0.0586(3) 0.5739(2) 0.0733(13) Uani 1 1 d . . . . .
H11A H 0.352184 -0.002416 0.567289 0.110 Uiso 1 1 calc GR . . . .
H11B H 0.381383 -0.052117 0.607274 0.110 Uiso 1 1 calc GR . . . .
H11C H 0.350048 -0.110614 0.576878 0.110 Uiso 1 1 calc GR . . . .
C13 C 0.38202(14) -0.0120(3) 0.32328(19) 0.0690(12) Uani 1 1 d . . . . .
H13 H 0.407334 -0.031835 0.328020 0.083 Uiso 1 1 calc R . . . .
C36 C 0.33481(14) 0.3387(3) 0.21364(18) 0.0689(12) Uani 1 1 d . . . . .
H36A H 0.313018 0.368457 0.198466 0.103 Uiso 1 1 calc GR . . . .
H36B H 0.338889 0.282978 0.193376 0.103 Uiso 1 1 calc GR . . . .
H36C H 0.354778 0.380744 0.211741 0.103 Uiso 1 1 calc GR . . . .
C56 C 0.42278(13) 0.1243(3) 0.6331(2) 0.0718(13) Uani 1 1 d . . . . .
H56A H 0.401375 0.105101 0.649060 0.108 Uiso 1 1 calc GR . . . .
H56B H 0.440509 0.075480 0.637496 0.108 Uiso 1 1 calc GR . . . .
H56C H 0.416986 0.136759 0.595058 0.108 Uiso 1 1 calc GR . . . .
C34 C 0.38256(18) 0.6917(3) 0.3422(3) 0.0913(17) Uani 1 1 d . . . . .
H34A H 0.382422 0.676317 0.304300 0.137 Uiso 1 1 calc GR . . . .
H34B H 0.404162 0.725773 0.353765 0.137 Uiso 1 1 calc GR . . . .
H34C H 0.361868 0.729471 0.347685 0.137 Uiso 1 1 calc GR . . . .
C2 C 0.32860(13) -0.0691(4) 0.3693(3) 0.0832(16) Uani 1 1 d . . . . .
H2 H 0.315482 -0.068172 0.335284 0.100 Uiso 1 1 calc R . . . .
C1 C 0.31174(13) -0.0949(4) 0.4135(3) 0.100(2) Uani 1 1 d . . . . .
C33 C 0.38160(15) 0.6225(5) 0.4358(2) 0.097(2) Uani 1 1 d . . . . .
H33A H 0.360418 0.657719 0.442088 0.146 Uiso 1 1 calc GR . . . .
H33B H 0.402734 0.658319 0.447502 0.146 Uiso 1 1 calc GR . . . .
H33C H 0.381832 0.565025 0.456027 0.146 Uiso 1 1 calc GR . . . .
C51 C 0.31426(12) 0.3234(5) 0.6948(2) 0.0859(17) Uani 1 1 d . . . . .
H51 H 0.318510 0.279879 0.725416 0.103 Uiso 1 1 calc R . . . .
C55 C 0.45030(15) 0.1958(4) 0.7218(3) 0.097(2) Uani 1 1 d . . . . .
H55A H 0.459589 0.252920 0.738101 0.146 Uiso 1 1 calc GR . . . .
H55B H 0.468890 0.148989 0.724673 0.146 Uiso 1 1 calc GR . . . .
H55C H 0.430232 0.174706 0.740394 0.146 Uiso 1 1 calc GR . . . .
C15 C 0.3658(2) -0.0539(4) 0.2696(3) 0.106(2) Uani 1 1 d . . . . .
H15A H 0.365816 -0.120887 0.272379 0.158 Uiso 1 1 calc GR . . . .
H15B H 0.379895 -0.035157 0.240803 0.158 Uiso 1 1 calc GR . . . .
H15C H 0.341463 -0.032009 0.261975 0.158 Uiso 1 1 calc GR . . . .
C14 C 0.3821(2) 0.0939(4) 0.3189(2) 0.0990(19) Uani 1 1 d . . . . .
H14A H 0.357843 0.116825 0.318856 0.148 Uiso 1 1 calc GR . . . .
H14B H 0.391745 0.111972 0.285648 0.148 Uiso 1 1 calc GR . . . .
H14C H 0.396727 0.119757 0.349340 0.148 Uiso 1 1 calc GR . . . .
C29 C 0.24796(14) 0.5437(5) 0.3579(4) 0.121(3) Uani 1 1 d . . . . .
H29 H 0.248803 0.612141 0.359915 0.145 Uiso 1 1 calc R . . . .
C31 C 0.21988(17) 0.5217(7) 0.3183(4) 0.149(4) Uani 1 1 d . . . . .
H31A H 0.226494 0.539809 0.283111 0.224 Uiso 1 1 calc GR . . . .
H31B H 0.198444 0.554673 0.326012 0.224 Uiso 1 1 calc GR . . . .
H31C H 0.215411 0.455590 0.318735 0.224 Uiso 1 1 calc GR . . . .
C7 C 0.27131(17) -0.1216(8) 0.4071(4) 0.163(4) Uani 1 1 d . . . . .
H7A H 0.263583 -0.140838 0.369710 0.196 Uiso 0.38(2) 1 calc R . P A 1
H7B H 0.272942 -0.151696 0.443001 0.196 Uiso 0.62(2) 1 calc R . P A 2
C30 C 0.24093(18) 0.5103(10) 0.4140(3) 0.185(6) Uani 1 1 d . . . . .
H30A H 0.239880 0.443198 0.414271 0.278 Uiso 1 1 calc GR . . . .
H30B H 0.218386 0.535318 0.423410 0.278 Uiso 1 1 calc GR . . . .
H30C H 0.260061 0.531124 0.440015 0.278 Uiso 1 1 calc GR . . . .
C8 C 0.24882(17) -0.0477(8) 0.4247(5) 0.174(5) Uani 1 1 d . . . . .
H8A H 0.253120 -0.040292 0.463506 0.261 Uiso 1 1 calc GR . . . .
H8B H 0.223911 -0.063217 0.415357 0.261 Uiso 1 1 calc GR . . . .
H8C H 0.254421 0.009646 0.407100 0.261 Uiso 1 1 calc GR . . . .
C9 C 0.2625(4) -0.2034(13) 0.4512(11) 0.114(10) Uani 0.38(2) 1 d . . P A 1
H9A H 0.277938 -0.256290 0.447133 0.170 Uiso 0.38(2) 1 calc GR . P A 1
H9B H 0.237748 -0.222341 0.444495 0.170 Uiso 0.38(2) 1 calc GR . P A 1
H9C H 0.266743 -0.179151 0.487526 0.170 Uiso 0.38(2) 1 calc GR . P A 1
C70 C 0.33386(16) 0.3391(4) 0.4765(4) 0.137(3) Uani 1 1 d . . . . .
H70A H 0.343594 0.374394 0.508130 0.164 Uiso 1 1 calc R . . . .
H70B H 0.334743 0.377816 0.444329 0.164 Uiso 1 1 calc R . . . .
C53 C 0.29460(19) 0.3970(5) 0.7112(4) 0.138(3) Uani 1 1 d . . . . .
H53A H 0.310460 0.441469 0.730272 0.206 Uiso 1 1 calc GR . . . .
H53B H 0.277411 0.374894 0.734979 0.206 Uiso 1 1 calc GR . . . .
H53C H 0.282076 0.426440 0.679937 0.206 Uiso 1 1 calc GR . . . .
C52 C 0.2900(2) 0.2721(7) 0.6473(4) 0.165(5) Uani 1 1 d . . . . .
H52A H 0.281771 0.316892 0.619922 0.248 Uiso 1 1 calc GR . . . .
H52B H 0.269621 0.243747 0.661948 0.248 Uiso 1 1 calc GR . . . .
H52C H 0.304040 0.224766 0.631446 0.248 Uiso 1 1 calc GR . . . .
C9A C 0.2629(3) -0.1979(10) 0.3829(11) 0.176(12) Uani 0.62(2) 1 d . . P A 2
H9AA H 0.266853 -0.192423 0.345084 0.265 Uiso 0.62(2) 1 calc GR . P A 2
H9AB H 0.237900 -0.211464 0.386076 0.265 Uiso 0.62(2) 1 calc GR . P A 2
H9AC H 0.277540 -0.247600 0.399145 0.265 Uiso 0.62(2) 1 calc GR . P A 2
C69 C 0.2978(2) 0.3102(7) 0.4824(5) 0.168(4) Uani 1 1 d . . . . .
H69A H 0.281034 0.342701 0.456434 0.202 Uiso 1 1 calc R . . . .
H69B H 0.291477 0.324171 0.518887 0.202 Uiso 1 1 calc R . . . .
C68 C 0.2960(2) 0.2073(7) 0.4724(6) 0.185(5) Uani 1 1 d . U . . .
H68A H 0.274521 0.190375 0.449154 0.222 Uiso 1 1 calc R . . . .
H68B H 0.296590 0.172503 0.506213 0.222 Uiso 1 1 calc R . . . .
C67 C 0.33041(17) 0.1909(6) 0.4436(4) 0.118(2) Uani 1 1 d . U . . .
H67A H 0.338963 0.127002 0.448149 0.141 Uiso 1 1 calc R . . . .
H67B H 0.326664 0.205532 0.405059 0.141 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.866(2) . ?
V1 O3 1.869(2) . ?
V1 O1 1.874(2) . ?
V1 O4 2.102(2) . ?
V1 N6 2.145(2) . ?
C9Ab H9AA 0.9600 . ?
C9Ab H9AB 0.9600 . ?
C9Ab H9AC 0.9600 . ?
O2 C43 1.355(3) . ?
O3 C65 1.346(4) . ?
O1 C21 1.351(4) . ?
O4 C70 1.440(6) . ?
O4 C67 1.389(7) . ?
N6 C22 1.497(4) . ?
N6 C66 1.500(4) . ?
N6 C44 1.491(4) . ?
C43 C42 1.406(4) . ?
C43 C38 1.407(4) . ?
C42 C41 1.391(4) . ?
C42 C44 1.505(4) . ?
C21 C20 1.405(4) . ?
C21 C16 1.405(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.396(4) . ?
C39 C40 1.386(4) . ?
C64 C65 1.411(4) . ?
C64 C63 1.399(4) . ?
C64 C66 1.489(4) . ?
C65 C60 1.400(4) . ?
C63 H63 0.9300 . ?
C63 C62 1.377(5) . ?
C38 C26 1.499(4) . ?
C26 C25 1.406(5) . ?
C26 C27 1.418(5) . ?
C48 C49 1.404(4) . ?
C48 C60 1.496(4) . ?
C48 C47 1.389(5) . ?
C49 C50 1.394(4) . ?
C49 C57 1.525(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C20 1.500(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.387(5) . ?
C61 H61 0.9300 . ?
C61 C60 1.398(4) . ?
C61 C62 1.393(4) . ?
C20 C19 1.395(4) . ?
C25 C24 1.387(5) . ?
C25 C32 1.503(5) . ?
C41 H41 0.9300 . ?
C47 C46 1.399(5) . ?
C47 C54 1.521(5) . ?
C16 C17 1.393(5) . ?
C16 C4 1.500(5) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C62 H62 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.388(5) . ?
C19 H19 0.9300 . ?
C19 C18 1.379(5) . ?
C50 H50 0.9300 . ?
C50 C45 1.387(5) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C57 H57 0.9800 . ?
C57 C59 1.535(5) . ?
C57 C58 1.533(5) . ?
C46 H46 0.9300 . ?
C46 C45 1.371(5) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C18 H18 0.9300 . ?
C4 C5 1.386(6) . ?
C4 C3 1.421(6) . ?
C45 C51 1.524(5) . ?
C5 C10 1.518(6) . ?
C5 C6 1.397(6) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.386(6) . ?
C32 H32 0.9800 . ?
C32 C34 1.542(7) . ?
C32 C33 1.509(6) . ?
C27 C35 1.518(5) . ?
C27 C28 1.392(5) . ?
C10 H10 0.9800 . ?
C10 C12 1.537(6) . ?
C10 C11 1.524(6) . ?
C35 H35 0.9800 . ?
C35 C37 1.534(5) . ?
C35 C36 1.527(6) . ?
C3 C13 1.510(7) . ?
C3 C2 1.391(6) . ?
C28 H28 0.9300 . ?
C28 C23 1.385(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C54 H54 0.9800 . ?
C54 C56 1.528(6) . ?
C54 C55 1.536(8) . ?
C23 C29 1.535(6) . ?
C6 H6 0.9300 . ?
C6 C1 1.415(9) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C15 1.524(6) . ?
C13 C14 1.517(6) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C2 H2 0.9300 . ?
C2 C1 1.357(9) . ?
C1 C7 1.546(7) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C51 H51 0.9800 . ?
C51 C53 1.364(8) . ?
C51 C52 1.589(10) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C29 H29 0.9800 . ?
C29 C31 1.397(11) . ?
C29 C30 1.508(12) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 C8 1.439(12) . ?
C7 C9 1.65(3) . ?
C7 C9A 1.269(15) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C70 C69 1.425(10) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C9A H9A 0.9600 . ?
C9A H9B 0.9600 . ?
C9A H9C 0.9600 . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C69 C68 1.492(12) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C68 C67 1.538(10) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O3 117.92(10) . . ?
H9AAb C9Ab H9AB 109.5 . . ?
H9AAb C9Ab H9AC 109.5 . . ?
O2 V1 O1 120.17(9) . . ?
O2 V1 O4 88.79(10) . . ?
O2 V1 N6 91.22(9) . . ?
O3 V1 O1 121.80(10) . . ?
O3 V1 O4 89.43(9) . . ?
H9ABb C9Ab H9AC 109.5 . . ?
C9Ab C7 C1 117.1(9) . . ?
C9Ab C7 H7B 92.3 . . ?
C9Ab C7 C8 130.4(8) . . ?
H9Ba C9A H9C 109.5 . . ?
O3 V1 N6 91.21(9) . . ?
O1 V1 O4 88.42(9) . . ?
O1 V1 N6 90.93(9) . . ?
O4 V1 N6 179.26(9) . . ?
C43 O2 V1 132.03(19) . . ?
C65 O3 V1 131.32(18) . . ?
C21 O1 V1 131.02(18) . . ?
C70 O4 V1 119.2(3) . . ?
C67 O4 V1 120.5(3) . . ?
C67 O4 C70 106.6(5) . . ?
C22 N6 V1 109.50(17) . . ?
C22 N6 C66 109.0(2) . . ?
C66 N6 V1 109.61(17) . . ?
C44 N6 V1 110.27(18) . . ?
C44 N6 C22 109.4(2) . . ?
C44 N6 C66 109.1(2) . . ?
O2 C43 C42 121.1(3) . . ?
O2 C43 C38 118.4(3) . . ?
C42 C43 C38 120.5(3) . . ?
C43 C42 C44 120.5(2) . . ?
C41 C42 C43 119.1(3) . . ?
C41 C42 C44 120.3(3) . . ?
O1 C21 C20 121.1(3) . . ?
O1 C21 C16 118.7(3) . . ?
C16 C21 C20 120.3(3) . . ?
C38 C39 H39 119.5 . . ?
C40 C39 H39 119.5 . . ?
C40 C39 C38 121.0(3) . . ?
C65 C64 C66 120.0(3) . . ?
C63 C64 C65 118.8(3) . . ?
C63 C64 C66 121.2(3) . . ?
O3 C65 C64 120.6(3) . . ?
O3 C65 C60 118.9(3) . . ?
C60 C65 C64 120.5(3) . . ?
C64 C63 H63 119.3 . . ?
C62 C63 C64 121.3(3) . . ?
C62 C63 H63 119.3 . . ?
C43 C38 C26 120.2(3) . . ?
C39 C38 C43 118.6(3) . . ?
C39 C38 C26 121.1(3) . . ?
C25 C26 C38 118.8(3) . . ?
C25 C26 C27 120.1(3) . . ?
C27 C26 C38 121.1(3) . . ?
C49 C48 C60 120.7(3) . . ?
C47 C48 C49 119.9(3) . . ?
C47 C48 C60 119.4(3) . . ?
C48 C49 C57 120.3(3) . . ?
C50 C49 C48 118.8(3) . . ?
C50 C49 C57 120.9(3) . . ?
N6 C22 H22A 108.9 . . ?
N6 C22 H22B 108.9 . . ?
N6 C22 C20 113.5(2) . . ?
H22A C22 H22B 107.7 . . ?
C20 C22 H22A 108.9 . . ?
C20 C22 H22B 108.9 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 119.9(3) . . ?
C41 C40 H40 120.0 . . ?
C60 C61 H61 119.4 . . ?
C62 C61 H61 119.4 . . ?
C62 C61 C60 121.3(3) . . ?
C21 C20 C22 119.9(3) . . ?
C19 C20 C21 119.3(3) . . ?
C19 C20 C22 120.8(3) . . ?
C26 C25 C32 122.1(3) . . ?
C24 C25 C26 118.7(3) . . ?
C24 C25 C32 119.2(3) . . ?
C65 C60 C48 119.6(3) . . ?
C61 C60 C65 118.8(3) . . ?
C61 C60 C48 121.5(3) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 C42 120.7(3) . . ?
C40 C41 H41 119.6 . . ?
C48 C47 C46 119.0(3) . . ?
C48 C47 C54 122.3(3) . . ?
C46 C47 C54 118.7(3) . . ?
C21 C16 C4 120.7(3) . . ?
C17 C16 C21 118.5(3) . . ?
C17 C16 C4 120.8(3) . . ?
N6 C66 H66A 108.7 . . ?
N6 C66 H66B 108.7 . . ?
C64 C66 N6 114.1(2) . . ?
C64 C66 H66A 108.7 . . ?
C64 C66 H66B 108.7 . . ?
H66A C66 H66B 107.6 . . ?
C63 C62 C61 119.4(3) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(3) . . ?
C18 C17 H17 119.2 . . ?
C20 C19 H19 119.5 . . ?
C18 C19 C20 120.9(3) . . ?
C18 C19 H19 119.5 . . ?
C49 C50 H50 118.9 . . ?
C45 C50 C49 122.2(3) . . ?
C45 C50 H50 118.9 . . ?
N6 C44 C42 114.4(2) . . ?
N6 C44 H44A 108.7 . . ?
N6 C44 H44B 108.7 . . ?
C42 C44 H44A 108.7 . . ?
C42 C44 H44B 108.7 . . ?
H44A C44 H44B 107.6 . . ?
C49 C57 H57 107.5 . . ?
C49 C57 C59 111.2(3) . . ?
C49 C57 C58 113.2(3) . . ?
C59 C57 H57 107.5 . . ?
C58 C57 H57 107.5 . . ?
C58 C57 C59 109.6(3) . . ?
C47 C46 H46 118.8 . . ?
C45 C46 C47 122.5(3) . . ?
C45 C46 H46 118.8 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.4(3) . . ?
C19 C18 H18 120.3 . . ?
C5 C4 C16 121.4(3) . . ?
C5 C4 C3 120.9(4) . . ?
C3 C4 C16 117.7(4) . . ?
C50 C45 C51 122.9(4) . . ?
C46 C45 C50 117.7(3) . . ?
C46 C45 C51 119.3(4) . . ?
C4 C5 C10 120.7(3) . . ?
C4 C5 C6 118.9(4) . . ?
C6 C5 C10 120.3(4) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C25 C24 H24 118.7 . . ?
C23 C24 C25 122.6(4) . . ?
C23 C24 H24 118.7 . . ?
C25 C32 H32 106.9 . . ?
C25 C32 C34 111.4(3) . . ?
C25 C32 C33 113.4(4) . . ?
C34 C32 H32 106.9 . . ?
C33 C32 H32 106.9 . . ?
C33 C32 C34 111.0(4) . . ?
C26 C27 C35 120.4(3) . . ?
C28 C27 C26 118.2(3) . . ?
C28 C27 C35 121.4(3) . . ?
C5 C10 H10 107.5 . . ?
C5 C10 C12 110.8(3) . . ?
C5 C10 C11 113.5(4) . . ?
C12 C10 H10 107.5 . . ?
C11 C10 H10 107.5 . . ?
C11 C10 C12 109.7(4) . . ?
C27 C35 H35 107.7 . . ?
C27 C35 C37 113.9(3) . . ?
C27 C35 C36 110.3(3) . . ?
C37 C35 H35 107.7 . . ?
C36 C35 H35 107.7 . . ?
C36 C35 C37 109.2(4) . . ?
C4 C3 C13 121.7(4) . . ?
C2 C3 C4 118.2(5) . . ?
C2 C3 C13 120.1(5) . . ?
C27 C28 H28 118.7 . . ?
C23 C28 C27 122.6(4) . . ?
C23 C28 H28 118.7 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C47 C54 H54 107.8 . . ?
C47 C54 C56 110.4(4) . . ?
C47 C54 C55 110.8(4) . . ?
C56 C54 H54 107.8 . . ?
C56 C54 C55 112.0(4) . . ?
C55 C54 H54 107.8 . . ?
C24 C23 C29 119.3(5) . . ?
C28 C23 C24 117.8(4) . . ?
C28 C23 C29 122.8(5) . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C1 120.5(5) . . ?
C1 C6 H6 119.8 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C3 C13 H13 106.8 . . ?
C3 C13 C15 115.2(5) . . ?
C3 C13 C14 111.4(4) . . ?
C15 C13 H13 106.8 . . ?
C14 C13 H13 106.8 . . ?
C14 C13 C15 109.4(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C3 C2 H2 119.0 . . ?
C1 C2 C3 122.1(5) . . ?
C1 C2 H2 119.0 . . ?
C6 C1 C7 120.3(7) . . ?
C2 C1 C6 119.4(5) . . ?
C2 C1 C7 120.3(7) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C45 C51 H51 108.3 . . ?
C45 C51 C52 107.3(4) . . ?
C53 C51 C45 117.4(5) . . ?
C53 C51 H51 108.3 . . ?
C53 C51 C52 106.9(7) . . ?
C52 C51 H51 108.3 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C23 C29 H29 106.1 . . ?
C31 C29 C23 115.1(6) . . ?
C31 C29 H29 106.1 . . ?
C31 C29 C30 112.8(7) . . ?
C30 C29 C23 110.0(6) . . ?
C30 C29 H29 106.1 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 C7 H7A 111.2 . . ?
C1 C7 H7B 92.3 . . ?
C1 C7 C9 111.1(10) . . ?
C8 C7 C1 112.1(7) . . ?
C8 C7 H7A 111.2 . . ?
C8 C7 H7B 92.3 . . ?
C8 C7 C9 99.5(10) . . ?
C9A C7 H7A 111.2 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
C7 C9Ab H9AA 109.5 . . ?
C7 C9Ab H9AB 109.5 . . ?
C7 C9Ab H9AC 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O4 C70 H70A 110.7 . . ?
O4 C70 H70B 110.7 . . ?
H70A C70 H70B 108.8 . . ?
C69 C70 O4 105.3(6) . . ?
C69 C70 H70A 110.7 . . ?
C69 C70 H70B 110.7 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C7 C9A H9A 109.5 . . ?
C7 C9A H9B 109.5 . . ?
C7 C9A H9C 109.5 . . ?
H9AA C9A H9B 109.5 . . ?
H9AA C9A H9C 109.5 . . ?
C70 C69 H69A 110.3 . . ?
C70 C69 H69B 110.3 . . ?
C70 C69 C68 107.2(6) . . ?
H69A C69 H69B 108.5 . . ?
C68 C69 H69A 110.3 . . ?
C68 C69 H69B 110.3 . . ?
C69 C68 H68A 111.4 . . ?
C69 C68 H68B 111.4 . . ?
C69 C68 C67 101.7(6) . . ?
H68A C68 H68B 109.3 . . ?
C67 C68 H68A 111.4 . . ?
C67 C68 H68B 111.4 . . ?
O4 C67 C68 100.7(6) . . ?
O4 C67 H67A 111.6 . . ?
O4 C67 H67B 111.6 . . ?
C68 C67 H67A 111.6 . . ?
C68 C67 H67B 111.6 . . ?
H67A C67 H67B 109.4 . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 172.0 electrons were 
found in a volume of 1164.0 A^3 in 3 voids. 
This is consistent with the presence of 
4 [n-pentane] per formula unit 
which account for 168.0 electrons.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.370 0.750 237.1 37.1 n-pentane
2 0.022 0.278 0.158 7.2 0.2 ?
3 -0.022 0.278 0.342 7.2 0.2 ?
4 0.000 0.630 0.250 237.1 37.1 n-pentane
5 0.022 0.722 0.658 7.2 0.2 ?
6 -0.022 0.722 0.842 7.2 0.2 ?
7 0.152 0.329 0.423 9.3 0.6 ?
8 0.152 0.671 0.923 9.3 0.6 ?
9 0.228 0.388 0.230 18.3 2.2 ?
10 0.228 0.612 0.730 18.3 2.2 ?
11 0.272 0.112 0.770 18.3 2.2 ?
12 0.272 0.888 0.270 18.3 2.2 ?
13 0.348 0.171 0.577 9.3 0.6 ?
14 0.348 0.829 0.077 9.3 0.6 ?
15 0.500 0.130 0.250 237.1 37.1 n-pentane
16 0.500 0.870 0.750 237.1 37.1 n-pentane
17 0.478 0.222 0.842 7.2 0.2 ?
18 0.478 0.778 0.342 7.2 0.2 ?
19 0.522 0.222 0.658 7.2 0.2 ?
20 0.522 0.778 0.158 7.2 0.2 ?
21 0.652 0.171 0.923 9.3 0.6 ?
22 0.652 0.829 0.423 9.3 0.6 ?
23 0.728 0.112 0.730 18.3 2.2 ?
24 0.728 0.888 0.230 18.3 2.2 ?
25 0.772 0.388 0.270 18.3 2.2 ?
26 0.772 0.612 0.770 18.3 2.2 ?
27 0.848 0.329 0.077 9.3 0.6 ?
28 0.848 0.671 0.577 9.3 0.6 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r-3
_database_code_depnum_ccdc_archive 'CCDC 1894391'
loop_
_audit_author_name
_audit_author_address
'Dae Young Bae'
;Pohang University of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
_audit_creation_date             2019-02-12
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.02.04 svn.r3569 for OlexSys, GUI svn.r5585)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C69 H91 N1 O4 Ti1, 3.5(C6 H6)'
_chemical_formula_sum            'C90 H112 N O4 Ti'
_chemical_formula_weight         1319.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   23.4039(2)
_cell_length_b                   23.4039(2)
_cell_length_c                   24.9083(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11815.5(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    38020
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.427
_cell_measurement_theta_min      1.295
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4278
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38020
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.427
_diffrn_reflns_theta_min         1.295
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7853
_reflns_number_total             12774
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.146
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         12774
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0784
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1422P)²+10.1453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2617
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-O2
 1.4248 with sigma of 0.02
 O2-C1A
 2.3732 with sigma of 0.04
 O2-C2
 2.4353 with sigma of 0.04
 C2-C1A
 2.5114 with sigma of 0.04
 C1-C2 \\sim C1-C1A
 with sigma of 0.02
 C2-C1 \\sim C1A-C1
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1A) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O2) = Uanis(O2) = Uanis(O2)
4. Rigid body (RIGU) restrains
 O2, C1, C2, C1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O2(0.33333) C1(0.33333) H1(0.33333) C2(0.33333) H2A(0.33333)
 H2B(0.33333) H2C(0.33333) C1A(0.33333) H1AA(0.33333) H1AB(0.33333)
 H1AC(0.33333)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C9(H9), C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C22(H22), C23(H23), C4(H4), C28(H28), C30(H30), C31(H31),
 C27(H27), C29(H29), C26(H26), C8(H8)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C1A(H1AA,
 H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.333333 0.666667 0.39457(2) 0.02054(11) Uani 1 3 d S T P . .
O1 O 0.34043(6) 0.59249(6) 0.40506(4) 0.0237(2) Uani 1 1 d . . . . .
N4 N 0.333333 0.666667 0.48768(8) 0.0170(3) Uani 1 3 d S T P A .
C20 C 0.32029(7) 0.55402(7) 0.49548(6) 0.0196(2) Uani 1 1 d . . . . .
C24 C 0.29223(7) 0.59787(7) 0.50825(5) 0.0195(2) Uani 1 1 d . . . . .
H24A H 0.248403 0.578757 0.492831 0.023 Uiso 1 1 calc R . . A .
H24B H 0.287921 0.599377 0.546884 0.023 Uiso 1 1 calc R . . . .
C21 C 0.32352(8) 0.51270(7) 0.53411(6) 0.0227(3) Uani 1 1 d . . . . .
H21 H 0.308295 0.512246 0.568678 0.027 Uiso 1 1 calc R . . . .
C19 C 0.34369(7) 0.55401(7) 0.44370(6) 0.0203(2) Uani 1 1 d . . . . .
C6 C 0.40429(8) 0.52421(8) 0.37731(6) 0.0236(3) Uani 1 1 d . . . . .
C5 C 0.46960(8) 0.57563(7) 0.36950(6) 0.0230(3) Uani 1 1 d . . . . .
C25 C 0.30931(9) 0.59898(9) 0.66676(7) 0.0300(3) Uani 1 1 d . . . . .
H25 H 0.293248 0.553724 0.667015 0.036 Uiso 1 1 calc R . . . .
C18 C 0.37302(7) 0.51598(7) 0.43118(6) 0.0221(3) Uani 1 1 d . . . . .
C12 C 0.50870(8) 0.62333(8) 0.41427(7) 0.0264(3) Uani 1 1 d . . . . .
H12 H 0.479120 0.612604 0.445162 0.032 Uiso 1 1 calc R . . . .
C22 C 0.34931(8) 0.47204(8) 0.52155(7) 0.0266(3) Uani 1 1 d . . . . .
H22 H 0.349476 0.443207 0.547164 0.032 Uiso 1 1 calc R . . . .
C23 C 0.37484(8) 0.47474(8) 0.47050(7) 0.0259(3) Uani 1 1 d . . . . .
H23 H 0.393354 0.448615 0.462605 0.031 Uiso 1 1 calc R . . . .
C4 C 0.49886(9) 0.58273(9) 0.31938(7) 0.0292(3) Uani 1 1 d . . . . .
H4 H 0.542366 0.615958 0.314407 0.035 Uiso 1 1 calc R . . . .
C7 C 0.36851(9) 0.48164(10) 0.33485(7) 0.0326(4) Uani 1 1 d . . . . .
C3 C 0.46471(10) 0.54139(10) 0.27649(7) 0.0334(4) Uani 1 1 d . . . . .
C28 C 0.12909(9) 0.43727(10) 0.66139(8) 0.0328(3) Uani 1 1 d . . . . .
H28 H 0.142207 0.421438 0.690326 0.039 Uiso 1 1 calc R . . . .
C30 C 0.06050(10) 0.47713(9) 0.62488(9) 0.0350(4) Uani 1 1 d . . . . .
H30 H 0.027084 0.487246 0.629254 0.042 Uiso 1 1 calc R . . . .
C31 C 0.09065(10) 0.48589(10) 0.57584(8) 0.0378(4) Uani 1 1 d . . . . .
H31 H 0.078232 0.502871 0.547250 0.045 Uiso 1 1 calc R . . . .
C27 C 0.15881(9) 0.44497(10) 0.61169(8) 0.0337(4) Uani 1 1 d . . . . .
H27 H 0.191428 0.433738 0.607165 0.040 Uiso 1 1 calc R . . . .
C13 C 0.56659(9) 0.61488(10) 0.43192(8) 0.0341(4) Uani 1 1 d . . . . .
H13A H 0.550378 0.570268 0.443521 0.051 Uiso 1 1 calc GR . . . .
H13B H 0.589455 0.644534 0.461012 0.051 Uiso 1 1 calc GR . . . .
H13C H 0.596313 0.624548 0.402309 0.051 Uiso 1 1 calc GR . . . .
C29 C 0.08002(10) 0.45311(10) 0.66796(8) 0.0344(4) Uani 1 1 d . . . . .
H29 H 0.059996 0.447693 0.701279 0.041 Uiso 1 1 calc R . . . .
C26 C 0.13982(10) 0.46943(10) 0.56874(8) 0.0367(4) Uani 1 1 d . . . . .
H26 H 0.159756 0.474835 0.535387 0.044 Uiso 1 1 calc R . . . .
C8 C 0.39969(10) 0.49126(11) 0.28502(7) 0.0367(4) Uani 1 1 d . . . . .
H8 H 0.376381 0.463402 0.256686 0.044 Uiso 1 1 calc R . . . .
C14 C 0.53212(10) 0.69500(9) 0.39871(9) 0.0367(4) Uani 1 1 d . . . . .
H14A H 0.564146 0.708235 0.370435 0.055 Uiso 1 1 calc GR . . . .
H14B H 0.551718 0.722986 0.429349 0.055 Uiso 1 1 calc GR . . . .
H14C H 0.495163 0.698697 0.386579 0.055 Uiso 1 1 calc GR . . . .
C15 C 0.29741(10) 0.42534(11) 0.34436(9) 0.0415(5) Uani 1 1 d . . . . .
H15 H 0.278941 0.439668 0.373202 0.050 Uiso 1 1 calc R . . . .
C9 C 0.49864(16) 0.55539(13) 0.22234(9) 0.0518(6) Uani 1 1 d . . . . .
H9 H 0.545576 0.572349 0.229517 0.062 Uiso 1 1 calc R . . . .
C10 C 0.47592(15) 0.49543(15) 0.18675(9) 0.0558(7) Uani 1 1 d . . . . .
H10A H 0.481006 0.462424 0.205529 0.084 Uiso 1 1 calc GR . . . .
H10B H 0.502013 0.507809 0.154590 0.084 Uiso 1 1 calc GR . . . .
H10C H 0.430347 0.478038 0.177567 0.084 Uiso 1 1 calc GR . . . .
C16 C 0.29521(12) 0.36138(12) 0.36389(12) 0.0525(6) Uani 1 1 d . . . . .
H16A H 0.310359 0.344229 0.335717 0.079 Uiso 1 1 calc GR . . . .
H16B H 0.250734 0.329218 0.373318 0.079 Uiso 1 1 calc GR . . . .
H16C H 0.323169 0.371075 0.394740 0.079 Uiso 1 1 calc GR . . . .
C17 C 0.25301(14) 0.41034(17) 0.29612(11) 0.0632(8) Uani 1 1 d . . . . .
H17A H 0.256092 0.450419 0.283171 0.095 Uiso 1 1 calc GR . . . .
H17B H 0.208247 0.379919 0.306195 0.095 Uiso 1 1 calc GR . . . .
H17C H 0.266486 0.391142 0.268345 0.095 Uiso 1 1 calc GR . . . .
C11 C 0.4937(3) 0.6103(2) 0.19453(14) 0.1129(17) Uani 1 1 d . U . . .
H11A H 0.448390 0.595645 0.186318 0.169 Uiso 1 1 calc GR . . . .
H11B H 0.518939 0.622036 0.161906 0.169 Uiso 1 1 calc GR . . . .
H11C H 0.510767 0.648076 0.217725 0.169 Uiso 1 1 calc GR . . . .
O2 O 0.3424(3) 0.6687(6) 0.32352(10) 0.0214(9) Uani 0.3333 1 d D U . A -1
C1 C 0.34679(13) 0.64073(19) 0.2747(3) 0.0541(13) Uani 0.3333 1 d D U . A -1
H1 H 0.364669 0.611260 0.280454 0.065 Uiso 0.3333 1 calc R . . A -1
C2 C 0.27428(18) 0.6014(6) 0.2479(3) 0.091(4) Uani 0.3333 1 d D U . A -1
H2A H 0.247529 0.561348 0.267520 0.137 Uiso 0.3333 1 calc GR . . A -1
H2B H 0.278034 0.590961 0.211280 0.137 Uiso 0.3333 1 calc GR . . A -1
H2C H 0.254175 0.628452 0.249069 0.137 Uiso 0.3333 1 calc GR . . A -1
C1A C 0.4012(4) 0.7090(2) 0.2471(3) 0.098(4) Uani 0.3333 1 d D U . A -1
H1AA H 0.418606 0.743446 0.273578 0.146 Uiso 0.3333 1 calc GR . . A -1
H1AB H 0.380937 0.720396 0.218752 0.146 Uiso 0.3333 1 calc GR . . A -1
H1AC H 0.436284 0.703700 0.232708 0.146 Uiso 0.3333 1 calc GR . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.8434(11) 3_565 y
Ti1 O1 1.8434(11) . y
Ti1 O1 1.8434(12) 2_665 y
Ti1 N4 2.319(2) . y
Ti1 O2 1.780(3) . y
O1 C19 1.3459(18) . ?
N4 C24 1.4939(15) 2_665 ?
N4 C24 1.4939(15) . ?
N4 C24 1.4939(15) 3_565 ?
C20 C24 1.503(2) . ?
C20 C21 1.393(2) . ?
C20 C19 1.4013(19) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C21 H21 0.9300 . ?
C21 C22 1.394(2) . ?
C19 C18 1.404(2) . ?
C6 C5 1.408(2) . ?
C6 C18 1.494(2) . ?
C6 C7 1.406(2) . ?
C5 C12 1.518(2) . ?
C5 C4 1.393(2) . ?
C25 C25 1.3910(18) 15_556 ?
C25 C25 1.3913(18) 14_456 ?
C25 H25 0.9300 . ?
C18 C23 1.391(2) . ?
C12 H12 0.9800 . ?
C12 C13 1.528(2) . ?
C12 C14 1.531(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.393(2) . ?
C23 H23 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.394(3) . ?
C7 C8 1.400(3) . ?
C7 C15 1.539(3) . ?
C3 C8 1.397(3) . ?
C3 C9 1.516(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.387(3) . ?
C28 C29 1.382(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.374(3) . ?
C30 C29 1.390(3) . ?
C31 H31 0.9300 . ?
C31 C26 1.396(3) . ?
C27 H27 0.9300 . ?
C27 C26 1.387(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C29 H29 0.9300 . ?
C26 H26 0.9300 . ?
C8 H8 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.550(4) . ?
C15 C17 1.510(3) . ?
C9 H9 0.9800 . ?
C9 C10 1.514(4) . ?
C9 C11 1.514(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
O2 C1 1.410(9) . ?
C1 H1 0.9800 . ?
C1 C2 1.615(5) . ?
C1 C1A 1.615(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 118.023(17) 3_565 2_665 y
O1 Ti1 O1 118.023(17) 3_565 . y
O1 Ti1 O1 118.024(17) 2_665 . y
O1 Ti1 N4 81.85(3) 3_565 . y
O1 Ti1 N4 81.85(3) . . y
O1 Ti1 N4 81.85(4) 2_665 . y
O2 Ti1 O1 95.8(4) . . y
O2 Ti1 O1 94.3(3) . 2_665 y
O2 Ti1 O1 104.29(19) . 3_565 y
O2 Ti1 N4 173.81(18) . . y
C19 O1 Ti1 142.51(10) . . ?
C24 N4 Ti1 110.06(9) 3_565 . ?
C24 N4 Ti1 110.06(9) 2_665 . ?
C24 N4 Ti1 110.06(9) . . ?
C24 N4 C24 108.87(9) 3_565 2_665 ?
C24 N4 C24 108.87(9) . 2_665 ?
C24 N4 C24 108.87(9) 3_565 . ?
C21 C20 C24 121.45(12) . . ?
C21 C20 C19 118.62(13) . . ?
C19 C20 C24 119.93(13) . . ?
N4 C24 C20 113.42(11) . . ?
N4 C24 H24A 108.9 . . ?
N4 C24 H24B 108.9 . . ?
C20 C24 H24A 108.9 . . ?
C20 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.77(14) . . ?
C22 C21 H21 119.6 . . ?
O1 C19 C20 120.34(13) . . ?
O1 C19 C18 118.34(13) . . ?
C20 C19 C18 121.28(14) . . ?
C5 C6 C18 119.13(13) . . ?
C7 C6 C5 120.59(14) . . ?
C7 C6 C18 120.28(14) . . ?
C6 C5 C12 121.63(13) . . ?
C4 C5 C6 118.98(15) . . ?
C4 C5 C12 119.40(15) . . ?
C25 C25 C25 119.991(3) 15_556 14_456 ?
C25 C25 H25 120.0 15_556 . ?
C25 C25 H25 120.0 14_456 . ?
C19 C18 C6 118.74(14) . . ?
C23 C18 C19 118.56(14) . . ?
C23 C18 C6 122.61(14) . . ?
C5 C12 H12 107.4 . . ?
C5 C12 C13 111.31(14) . . ?
C5 C12 C14 111.92(15) . . ?
C13 C12 H12 107.4 . . ?
C13 C12 C14 111.07(15) . . ?
C14 C12 H12 107.4 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.75(15) . . ?
C23 C22 H22 120.1 . . ?
C18 C23 C22 120.86(14) . . ?
C18 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C5 C4 H4 119.1 . . ?
C5 C4 C3 121.79(17) . . ?
C3 C4 H4 119.1 . . ?
C6 C7 C15 119.78(15) . . ?
C8 C7 C6 118.36(17) . . ?
C8 C7 C15 121.84(16) . . ?
C4 C3 C8 118.18(15) . . ?
C4 C3 C9 118.4(2) . . ?
C8 C3 C9 123.35(19) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C29 C28 C27 120.08(17) . . ?
C31 C30 H30 120.0 . . ?
C31 C30 C29 119.92(18) . . ?
C29 C30 H30 120.0 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C26 120.28(18) . . ?
C26 C31 H31 119.9 . . ?
C28 C27 H27 120.1 . . ?
C28 C27 C26 119.90(18) . . ?
C26 C27 H27 120.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C28 C29 C30 120.14(18) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C26 H26 120.2 . . ?
C27 C26 C31 119.66(18) . . ?
C27 C26 H26 120.2 . . ?
C7 C8 H8 119.0 . . ?
C3 C8 C7 122.08(17) . . ?
C3 C8 H8 119.0 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 H15 107.0 . . ?
C7 C15 C16 112.00(18) . . ?
C16 C15 H15 107.0 . . ?
C17 C15 C7 113.6(2) . . ?
C17 C15 H15 107.0 . . ?
C17 C15 C16 109.8(2) . . ?
C3 C9 H9 106.6 . . ?
C10 C9 C3 114.7(2) . . ?
C10 C9 H9 106.6 . . ?
C10 C9 C11 112.2(3) . . ?
C11 C9 C3 109.7(2) . . ?
C11 C9 H9 106.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 O2 Ti1 151.7(8) . . ?
O2 C1 H1 110.9 . . ?
O2 C1 C2 108.7(4) . . ?
O2 C1 C1A 96.4(5) . . ?
C2 C1 H1 110.9 . . ?
C2 C1 C1A 118.2(7) . . ?
C1A C1 H1 110.9 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C1A H1AA 109.5 . . ?
C1 C1A H1AB 109.5 . . ?
C1 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O1 C19 C20 21.2(2) . . . . ?
Ti1 O1 C19 C18 -156.62(13) . . . . ?
Ti1 N4 C24 C20 66.19(11) . . . . ?
Ti1 O2 C1 C2 94.5(10) . . . . ?
Ti1 O2 C1 C1A -142.8(9) . . . . ?
O1 Ti1 O1 C19 76.76(16) 2_665 . . . ?
O1 Ti1 O1 C19 -75.64(17) 3_565 . . . ?
O1 Ti1 O2 C1 8.4(9) . . . . ?
O1 Ti1 O2 C1 127.2(9) 2_665 . . . ?
O1 Ti1 O2 C1 -112.4(8) 3_565 . . . ?
O1 C19 C18 C6 5.2(2) . . . . ?
O1 C19 C18 C23 -178.21(13) . . . . ?
N4 Ti1 O1 C19 0.56(16) . . . . ?
C20 C21 C22 C23 2.8(2) . . . . ?
C20 C19 C18 C6 -172.68(13) . . . . ?
C20 C19 C18 C23 3.9(2) . . . . ?
C24 N4 C24 C20 -54.5(2) 2_665 . . . ?
C24 N4 C24 C20 -173.09(10) 3_565 . . . ?
C24 C20 C21 C22 179.60(14) . . . . ?
C24 C20 C19 O1 -0.8(2) . . . . ?
C24 C20 C19 C18 176.96(13) . . . . ?
C21 C20 C24 N4 134.50(15) . . . . ?
C21 C20 C19 O1 178.94(13) . . . . ?
C21 C20 C19 C18 -3.3(2) . . . . ?
C21 C22 C23 C18 -2.1(3) . . . . ?
C19 C20 C24 N4 -45.73(19) . . . . ?
C19 C20 C21 C22 -0.2(2) . . . . ?
C19 C18 C23 C22 -1.2(2) . . . . ?
C6 C5 C12 C13 113.23(17) . . . . ?
C6 C5 C12 C14 -121.81(17) . . . . ?
C6 C5 C4 C3 1.6(2) . . . . ?
C6 C18 C23 C22 175.28(15) . . . . ?
C6 C7 C8 C3 0.1(3) . . . . ?
C6 C7 C15 C16 -88.8(2) . . . . ?
C6 C7 C15 C17 146.2(2) . . . . ?
C5 C6 C18 C19 84.06(19) . . . . ?
C5 C6 C18 C23 -92.43(19) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C5 C6 C7 C15 179.43(17) . . . . ?
C5 C4 C3 C8 -0.8(3) . . . . ?
C5 C4 C3 C9 175.90(18) . . . . ?
C18 C6 C5 C12 -0.7(2) . . . . ?
C18 C6 C5 C4 179.31(14) . . . . ?
C18 C6 C7 C8 179.82(17) . . . . ?
C18 C6 C7 C15 -1.4(3) . . . . ?
C12 C5 C4 C3 -178.37(16) . . . . ?
C4 C5 C12 C13 -66.8(2) . . . . ?
C4 C5 C12 C14 58.2(2) . . . . ?
C4 C3 C8 C7 -0.1(3) . . . . ?
C4 C3 C9 C10 152.2(2) . . . . ?
C4 C3 C9 C11 -80.4(4) . . . . ?
C7 C6 C5 C12 178.43(15) . . . . ?
C7 C6 C5 C4 -1.6(2) . . . . ?
C7 C6 C18 C19 -95.09(19) . . . . ?
C7 C6 C18 C23 88.4(2) . . . . ?
C28 C27 C26 C31 -0.3(3) . . . . ?
C30 C31 C26 C27 -0.9(3) . . . . ?
C31 C30 C29 C28 -0.8(3) . . . . ?
C27 C28 C29 C30 -0.3(3) . . . . ?
C29 C28 C27 C26 0.9(3) . . . . ?
C29 C30 C31 C26 1.4(3) . . . . ?
C8 C7 C15 C16 89.9(3) . . . . ?
C8 C7 C15 C17 -35.2(3) . . . . ?
C8 C3 C9 C10 -31.2(3) . . . . ?
C8 C3 C9 C11 96.1(3) . . . . ?
C15 C7 C8 C3 -178.6(2) . . . . ?
C9 C3 C8 C7 -176.6(2) . . . . ?
O2 Ti1 O1 C19 174.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p21c
_database_code_depnum_ccdc_archive 'CCDC 1894389'
loop_
_audit_author_name
_audit_author_address
'Dae Young Bae'
;Pohang University of Science and Technology
South Korea
;
_audit_update_record             
;
2019-01-29 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_p21c                
;
PROBLEM: D-H Without Acceptor O1 -- H1
RESPONSE: There are no proper acceptors for this H atom.
;
# end Validation Reply Form

_audit_creation_date             2018-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H87 N O3, C4 H8 O'
_chemical_formula_sum            'C70 H95 N O4'
_chemical_formula_weight         1014.46
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.089(4)
_cell_length_b                   9.862(2)
_cell_length_c                   27.858(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.81(3)
_cell_angle_gamma                90
_cell_volume                     6055(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    37868
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.465
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.995
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37868
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.465
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_source                   'PLSII 2D bending magnet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6568
_reflns_number_total             10276
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0621
_refine_ls_restrained_S_all      0.792
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2247
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C54(H54), C29(H29), C57(H57), C51(H51), C32(H32),
 C35(H35), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C22(H22A,H22B), C44(H44A,H44B), C70(H70A,H70B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B)
2.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C61(H61), C62(H62), C19(H19), C46(H46), C50(H50), C18(H18),
 C24(H24), C17(H17), C6(H6), C28(H28), C2(H2A), C41(H41), C43(H43), C42(H42)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C56(H56A,H56B,H56C), C14(H14A,H14B,H14C), C55(H55A,H55B,
 H55C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C58(H58A,H58B,H58C), C36(H36A,
 H36B,H36C), C30(H30A,H30B,H30C), C59(H59A,H59B,H59C), C8(H8A,H8B,H8C),
 C52(H52A,H52B,H52C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C53(H53A,H53B,H53C),
  C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.83998(9) 0.33475(18) 0.21819(7) 0.0337(5) Uani 1 1 d . . . . .
O3 O 0.68039(8) 0.28682(18) 0.37270(7) 0.0343(4) Uani 1 1 d . . . . .
H3 H 0.716403 0.259223 0.373231 0.051 Uiso 1 1 calc GR . . . .
O2 O 0.79576(9) 0.23330(18) 0.44059(7) 0.0387(5) Uani 1 1 d . . . . .
H2 H 0.792407 0.274690 0.466636 0.058 Uiso 1 1 calc GR . . . .
N1 N 0.77604(9) 0.14614(19) 0.34027(7) 0.0279(5) Uani 1 1 d . . . . .
O4 O 0.76197(13) 0.4707(3) 0.48507(9) 0.0694(7) Uani 1 1 d . . . . .
C64 C 0.66758(11) 0.1019(2) 0.31672(9) 0.0289(6) Uani 1 1 d . . . . .
C21 C 0.84430(11) 0.4069(3) 0.26030(9) 0.0287(6) Uani 1 1 d . . . . .
C65 C 0.64656(11) 0.2218(2) 0.33706(9) 0.0289(6) Uani 1 1 d . . . . .
C20 C 0.81940(11) 0.3471(2) 0.30015(9) 0.0287(6) Uani 1 1 d . . . . .
C60 C 0.59103(12) 0.2800(2) 0.32093(10) 0.0300(6) Uani 1 1 d . . . . .
C39 C 0.81389(12) 0.1042(3) 0.44991(10) 0.0324(6) Uani 1 1 d . . . . .
C63 C 0.63093(12) 0.0395(2) 0.28043(10) 0.0319(6) Uani 1 1 d . . . . .
H63 H 0.644399 -0.041986 0.266417 0.038 Uiso 1 1 calc R . . . .
C4 C 0.89824(12) 0.5950(2) 0.21902(9) 0.0305(6) Uani 1 1 d . . . . .
C66 C 0.72798(11) 0.0415(2) 0.33377(10) 0.0305(6) Uani 1 1 d . . . . .
H66A H 0.723818 -0.005799 0.364718 0.037 Uiso 1 1 calc R . . . .
H66B H 0.740083 -0.026329 0.310044 0.037 Uiso 1 1 calc R . . . .
C16 C 0.87155(11) 0.5349(2) 0.26304(9) 0.0297(6) Uani 1 1 d . . . . .
C48 C 0.56916(11) 0.4114(2) 0.34113(10) 0.0307(6) Uani 1 1 d . . . . .
C61 C 0.55604(12) 0.2129(3) 0.28462(10) 0.0330(6) Uani 1 1 d . . . . .
H61 H 0.517980 0.250211 0.273542 0.040 Uiso 1 1 calc R . . . .
C22 C 0.78746(12) 0.2120(2) 0.29422(9) 0.0307(6) Uani 1 1 d . . . . .
H22A H 0.748233 0.225665 0.275518 0.037 Uiso 1 1 calc R . . . .
H22B H 0.812419 0.150727 0.275475 0.037 Uiso 1 1 calc R . . . .
C62 C 0.57538(12) 0.0936(3) 0.26437(10) 0.0336(6) Uani 1 1 d . . . . .
H62 H 0.550866 0.049459 0.239783 0.040 Uiso 1 1 calc R . . . .
C38 C 0.81460(12) 0.0484(3) 0.49583(10) 0.0352(6) Uani 1 1 d . . . . .
C45 C 0.52100(12) 0.6580(3) 0.37259(10) 0.0357(6) Uani 1 1 d . . . . .
C5 C 0.86101(12) 0.6640(2) 0.18432(10) 0.0320(6) Uani 1 1 d . . . . .
C19 C 0.82357(12) 0.4181(3) 0.34334(10) 0.0334(6) Uani 1 1 d . . . . .
H19 H 0.807761 0.378682 0.371005 0.040 Uiso 1 1 calc R . . . .
C3 C 0.96095(12) 0.5833(3) 0.21343(10) 0.0349(6) Uani 1 1 d . . . . .
C47 C 0.59369(12) 0.5346(3) 0.32704(10) 0.0322(6) Uani 1 1 d . . . . .
C40 C 0.83124(12) 0.0281(3) 0.41065(10) 0.0331(6) Uani 1 1 d . . . . .
C23 C 0.74365(13) 0.2470(3) 0.61743(10) 0.0369(7) Uani 1 1 d . . . . .
C13 C 0.79332(12) 0.6822(3) 0.19003(10) 0.0342(6) Uani 1 1 d . . . . .
H13 H 0.780842 0.611351 0.213070 0.041 Uiso 1 1 calc R . . . .
C46 C 0.56907(13) 0.6552(3) 0.34276(10) 0.0364(7) Uani 1 1 d . . . . .
H46 H 0.585659 0.738626 0.332772 0.044 Uiso 1 1 calc R . . . .
C27 C 0.82908(13) 0.1969(3) 0.56964(10) 0.0365(6) Uani 1 1 d . . . . .
C49 C 0.52187(12) 0.4116(3) 0.37251(10) 0.0357(6) Uani 1 1 d . . . . .
C44 C 0.83285(12) 0.0880(3) 0.36122(10) 0.0326(6) Uani 1 1 d . . . . .
H44A H 0.864192 0.159937 0.362372 0.039 Uiso 1 1 calc R . . . .
H44B H 0.845985 0.016447 0.339275 0.039 Uiso 1 1 calc R . . . .
C10 C 1.00196(13) 0.5056(3) 0.24952(11) 0.0390(7) Uani 1 1 d . . . . .
H10 H 0.975553 0.441790 0.266599 0.047 Uiso 1 1 calc R . . . .
C54 C 0.64482(13) 0.5424(3) 0.29272(10) 0.0374(7) Uani 1 1 d . . . . .
H54 H 0.660754 0.448687 0.288094 0.045 Uiso 1 1 calc R . . . .
C50 C 0.49914(13) 0.5351(3) 0.38753(10) 0.0372(7) Uani 1 1 d . . . . .
H50 H 0.467360 0.534677 0.408896 0.045 Uiso 1 1 calc R . . . .
C18 C 0.85032(13) 0.5453(3) 0.34692(10) 0.0364(6) Uani 1 1 d . . . . .
H18 H 0.852569 0.592537 0.376700 0.044 Uiso 1 1 calc R . . . .
C24 C 0.70644(13) 0.1802(3) 0.58362(10) 0.0388(7) Uani 1 1 d . . . . .
H24 H 0.664230 0.175794 0.588110 0.047 Uiso 1 1 calc R . . . .
C26 C 0.79075(13) 0.1248(3) 0.53689(10) 0.0356(6) Uani 1 1 d . . . . .
C17 C 0.87367(12) 0.6028(3) 0.30683(10) 0.0343(6) Uani 1 1 d . . . . .
H17 H 0.891513 0.690387 0.309266 0.041 Uiso 1 1 calc R . . . .
C6 C 0.88671(13) 0.7215(3) 0.14475(11) 0.0378(7) Uani 1 1 d . . . . .
H6 H 0.861274 0.768652 0.121522 0.045 Uiso 1 1 calc R . . . .
C29 C 0.71746(13) 0.3098(3) 0.66164(10) 0.0394(7) Uani 1 1 d . . . . .
H29 H 0.751818 0.348044 0.682587 0.047 Uiso 1 1 calc R . . . .
C28 C 0.80493(13) 0.2559(3) 0.60973(10) 0.0361(6) Uani 1 1 d . . . . .
H28 H 0.831155 0.303283 0.632344 0.043 Uiso 1 1 calc R . . . .
C2 C 0.98429(13) 0.6442(3) 0.17312(11) 0.0401(7) Uani 1 1 d . . . . .
H2A H 1.026677 0.638923 0.169436 0.048 Uiso 1 1 calc R . . . .
C25 C 0.72786(13) 0.1190(3) 0.54332(10) 0.0392(7) Uani 1 1 d . . . . .
C41 C 0.85062(14) -0.1050(3) 0.41900(11) 0.0425(7) Uani 1 1 d . . . . .
H41 H 0.862220 -0.158417 0.392764 0.051 Uiso 1 1 calc R . . . .
C1 C 0.94771(13) 0.7121(3) 0.13827(11) 0.0409(7) Uani 1 1 d . . . . .
C57 C 0.49384(13) 0.2829(3) 0.39061(12) 0.0442(8) Uani 1 1 d . . . . .
H57 H 0.518727 0.204596 0.380427 0.053 Uiso 1 1 calc R . . . .
C51 C 0.49387(13) 0.7903(3) 0.38849(11) 0.0407(7) Uani 1 1 d . . . . .
H51 H 0.454647 0.768028 0.402666 0.049 Uiso 1 1 calc R . . . .
C43 C 0.83500(14) -0.0844(3) 0.50230(11) 0.0456(7) Uani 1 1 d . . . . .
H43 H 0.836301 -0.123299 0.533550 0.055 Uiso 1 1 calc R . . . .
C31 C 0.68676(13) 0.1988(3) 0.69020(11) 0.0422(7) Uani 1 1 d . . . . .
H31A H 0.656283 0.152045 0.669064 0.063 Uiso 1 1 calc GR . . . .
H31B H 0.667073 0.240197 0.717103 0.063 Uiso 1 1 calc GR . . . .
H31C H 0.717358 0.133563 0.702657 0.063 Uiso 1 1 calc GR . . . .
C32 C 0.68432(14) 0.0455(3) 0.50813(11) 0.0460(8) Uani 1 1 d . . . . .
H32 H 0.708086 0.006998 0.481999 0.055 Uiso 1 1 calc R . . . .
C56 C 0.62070(14) 0.5963(3) 0.24421(11) 0.0465(8) Uani 1 1 d . . . . .
H56A H 0.587995 0.537318 0.230991 0.070 Uiso 1 1 calc GR . . . .
H56B H 0.653512 0.598139 0.222211 0.070 Uiso 1 1 calc GR . . . .
H56C H 0.604991 0.688319 0.248065 0.070 Uiso 1 1 calc GR . . . .
C14 C 0.78164(14) 0.8193(3) 0.21233(12) 0.0479(8) Uani 1 1 d . . . . .
H14A H 0.803883 0.825439 0.243887 0.072 Uiso 1 1 calc GR . . . .
H14B H 0.738108 0.829855 0.216137 0.072 Uiso 1 1 calc GR . . . .
H14C H 0.795403 0.891279 0.191365 0.072 Uiso 1 1 calc GR . . . .
C55 C 0.69706(13) 0.6315(3) 0.31300(12) 0.0471(8) Uani 1 1 d . . . . .
H55A H 0.682498 0.724498 0.316849 0.071 Uiso 1 1 calc GR . . . .
H55B H 0.729689 0.631113 0.290822 0.071 Uiso 1 1 calc GR . . . .
H55C H 0.712487 0.596094 0.344331 0.071 Uiso 1 1 calc GR . . . .
C35 C 0.89621(13) 0.2130(3) 0.56242(11) 0.0450(7) Uani 1 1 d . . . . .
H35 H 0.906057 0.153004 0.535063 0.054 Uiso 1 1 calc R . . . .
C42 C 0.85331(15) -0.1607(3) 0.46454(12) 0.0499(8) Uani 1 1 d . . . . .
H42 H 0.867648 -0.250640 0.469748 0.060 Uiso 1 1 calc R . . . .
C15 C 0.75465(14) 0.6626(3) 0.14315(11) 0.0473(8) Uani 1 1 d . . . . .
H15A H 0.763426 0.735125 0.120591 0.071 Uiso 1 1 calc GR . . . .
H15B H 0.711611 0.665419 0.149648 0.071 Uiso 1 1 calc GR . . . .
H15C H 0.764071 0.574627 0.129082 0.071 Uiso 1 1 calc GR . . . .
C7 C 0.97447(14) 0.7708(3) 0.09305(12) 0.0484(8) Uani 1 1 d . . . . .
H7 H 0.940638 0.816698 0.073696 0.058 Uiso 1 1 calc R . . . .
C12 C 1.04871(14) 0.4201(3) 0.22580(12) 0.0465(8) Uani 1 1 d . . . . .
H12A H 1.028465 0.365302 0.200126 0.070 Uiso 1 1 calc GR . . . .
H12B H 1.069140 0.360158 0.249822 0.070 Uiso 1 1 calc GR . . . .
H12C H 1.078690 0.479472 0.212130 0.070 Uiso 1 1 calc GR . . . .
C58 C 0.42998(14) 0.2648(3) 0.36845(12) 0.0478(8) Uani 1 1 d . . . . .
H58A H 0.404491 0.339707 0.378391 0.072 Uiso 1 1 calc GR . . . .
H58B H 0.413446 0.178677 0.379284 0.072 Uiso 1 1 calc GR . . . .
H58C H 0.430627 0.264234 0.333308 0.072 Uiso 1 1 calc GR . . . .
C36 C 0.93555(14) 0.1687(4) 0.60643(12) 0.0525(8) Uani 1 1 d . . . . .
H36A H 0.928325 0.228795 0.633482 0.079 Uiso 1 1 calc GR . . . .
H36B H 0.978385 0.173468 0.599408 0.079 Uiso 1 1 calc GR . . . .
H36C H 0.925317 0.075343 0.614793 0.079 Uiso 1 1 calc GR . . . .
C30 C 0.67386(15) 0.4237(3) 0.64821(12) 0.0503(8) Uani 1 1 d . . . . .
H30A H 0.694386 0.492148 0.629642 0.075 Uiso 1 1 calc GR . . . .
H30B H 0.659995 0.465132 0.677510 0.075 Uiso 1 1 calc GR . . . .
H30C H 0.638897 0.387648 0.628763 0.075 Uiso 1 1 calc GR . . . .
C59 C 0.49387(15) 0.2806(3) 0.44563(12) 0.0553(9) Uani 1 1 d . . . . .
H59A H 0.534236 0.305399 0.459609 0.083 Uiso 1 1 calc GR . . . .
H59B H 0.483511 0.189303 0.456331 0.083 Uiso 1 1 calc GR . . . .
H59C H 0.463881 0.345515 0.456136 0.083 Uiso 1 1 calc GR . . . .
C8 C 0.99862(17) 0.6600(4) 0.06197(12) 0.0601(10) Uani 1 1 d . . . . .
H8A H 1.032282 0.613459 0.079767 0.090 Uiso 1 1 calc GR . . . .
H8B H 1.013018 0.699978 0.032603 0.090 Uiso 1 1 calc GR . . . .
H8C H 0.966200 0.594806 0.053412 0.090 Uiso 1 1 calc GR . . . .
C52 C 0.47989(17) 0.8857(3) 0.34798(13) 0.0570(9) Uani 1 1 d . . . . .
H52A H 0.517816 0.917863 0.335582 0.085 Uiso 1 1 calc GR . . . .
H52B H 0.456999 0.963114 0.359362 0.085 Uiso 1 1 calc GR . . . .
H52C H 0.455625 0.839037 0.322283 0.085 Uiso 1 1 calc GR . . . .
C9 C 1.02148(16) 0.8749(4) 0.10526(13) 0.0607(9) Uani 1 1 d . . . . .
H9A H 1.002813 0.952986 0.120224 0.091 Uiso 1 1 calc GR . . . .
H9B H 1.039807 0.904038 0.075881 0.091 Uiso 1 1 calc GR . . . .
H9C H 1.052895 0.836301 0.127735 0.091 Uiso 1 1 calc GR . . . .
C70 C 0.72920(18) 0.5414(4) 0.44758(13) 0.0635(10) Uani 1 1 d . . . . .
H70A H 0.727232 0.487341 0.417578 0.076 Uiso 1 1 calc R . . . .
H70B H 0.749031 0.629170 0.441405 0.076 Uiso 1 1 calc R . . . .
C37 C 0.90991(17) 0.3594(4) 0.54819(15) 0.0710(11) Uani 1 1 d . . . . .
H37A H 0.884711 0.383815 0.519190 0.107 Uiso 1 1 calc GR . . . .
H37B H 0.952849 0.367444 0.541768 0.107 Uiso 1 1 calc GR . . . .
H37C H 0.900928 0.420615 0.574504 0.107 Uiso 1 1 calc GR . . . .
C53 C 0.5342(2) 0.8552(4) 0.42737(15) 0.0764(12) Uani 1 1 d . . . . .
H53A H 0.543211 0.789659 0.453316 0.115 Uiso 1 1 calc GR . . . .
H53B H 0.513611 0.934134 0.440105 0.115 Uiso 1 1 calc GR . . . .
H53C H 0.572089 0.884127 0.414099 0.115 Uiso 1 1 calc GR . . . .
C11 C 1.03282(18) 0.5962(4) 0.28730(15) 0.0700(11) Uani 1 1 d . . . . .
H11A H 1.060291 0.658558 0.272056 0.105 Uiso 1 1 calc GR . . . .
H11B H 1.056059 0.540603 0.311142 0.105 Uiso 1 1 calc GR . . . .
H11C H 1.002171 0.648418 0.303238 0.105 Uiso 1 1 calc GR . . . .
C34 C 0.6531(2) -0.0711(4) 0.53238(15) 0.0782(13) Uani 1 1 d . . . . .
H34A H 0.683769 -0.134048 0.546365 0.117 Uiso 1 1 calc GR . . . .
H34B H 0.626397 -0.119024 0.508534 0.117 Uiso 1 1 calc GR . . . .
H34C H 0.629057 -0.035397 0.557860 0.117 Uiso 1 1 calc GR . . . .
C33 C 0.63652(19) 0.1425(4) 0.48507(15) 0.0717(11) Uani 1 1 d . . . . .
H33A H 0.612839 0.181772 0.510150 0.108 Uiso 1 1 calc GR . . . .
H33B H 0.609442 0.092531 0.462067 0.108 Uiso 1 1 calc GR . . . .
H33C H 0.656752 0.215184 0.468272 0.108 Uiso 1 1 calc GR . . . .
C67 C 0.7415(2) 0.5255(4) 0.52755(14) 0.0762(12) Uani 1 1 d . . . . .
H67A H 0.760346 0.615043 0.534612 0.091 Uiso 1 1 calc R . . . .
H67B H 0.751056 0.464291 0.555189 0.091 Uiso 1 1 calc R . . . .
C68 C 0.6729(2) 0.5391(5) 0.51715(17) 0.0868(14) Uani 1 1 d . . . . .
H68A H 0.651854 0.454732 0.525745 0.104 Uiso 1 1 calc R . . . .
H68B H 0.656723 0.615507 0.535463 0.104 Uiso 1 1 calc R . . . .
C69 C 0.6650(2) 0.5648(6) 0.46449(17) 0.1059(18) Uani 1 1 d . . . . .
H69A H 0.651209 0.658805 0.457757 0.127 Uiso 1 1 calc R . . . .
H69B H 0.635507 0.500791 0.448658 0.127 Uiso 1 1 calc R . . . .
H1 H 0.859(2) 0.379(4) 0.1983(16) 0.086(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C21 1.370(3) . ?
O1 H1 0.84(4) . ?
O3 H3 0.8400 . ?
O3 C65 1.362(3) . ?
O2 H2 0.8400 . ?
O2 C39 1.355(3) . ?
N1 C66 1.483(3) . ?
N1 C22 1.475(3) . ?
N1 C44 1.465(3) . ?
O4 C70 1.415(4) . ?
O4 C67 1.403(4) . ?
C64 C65 1.404(3) . ?
C64 C63 1.395(4) . ?
C64 C66 1.508(4) . ?
C21 C20 1.401(3) . ?
C21 C16 1.398(4) . ?
C65 C60 1.401(4) . ?
C20 C22 1.511(3) . ?
C20 C19 1.390(4) . ?
C60 C48 1.505(3) . ?
C60 C61 1.398(4) . ?
C39 C38 1.392(4) . ?
C39 C40 1.400(4) . ?
C63 H63 0.9500 . ?
C63 C62 1.385(4) . ?
C4 C16 1.516(3) . ?
C4 C5 1.403(4) . ?
C4 C3 1.409(4) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C16 C17 1.390(4) . ?
C48 C47 1.398(4) . ?
C48 C49 1.406(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.385(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C62 H62 0.9500 . ?
C38 C26 1.495(4) . ?
C38 C43 1.393(4) . ?
C45 C46 1.391(4) . ?
C45 C50 1.380(4) . ?
C45 C51 1.514(4) . ?
C5 C13 1.525(4) . ?
C5 C6 1.394(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.387(4) . ?
C3 C10 1.516(4) . ?
C3 C2 1.401(4) . ?
C47 C46 1.390(4) . ?
C47 C54 1.529(4) . ?
C40 C44 1.501(4) . ?
C40 C41 1.395(4) . ?
C23 C24 1.376(4) . ?
C23 C29 1.526(4) . ?
C23 C28 1.387(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.517(4) . ?
C13 C15 1.524(4) . ?
C46 H46 0.9500 . ?
C27 C26 1.397(4) . ?
C27 C28 1.396(4) . ?
C27 C35 1.518(4) . ?
C49 C50 1.393(4) . ?
C49 C57 1.513(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C10 H10 1.0000 . ?
C10 C12 1.519(4) . ?
C10 C11 1.508(5) . ?
C54 H54 1.0000 . ?
C54 C56 1.516(4) . ?
C54 C55 1.529(4) . ?
C50 H50 0.9500 . ?
C18 H18 0.9500 . ?
C18 C17 1.383(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.385(4) . ?
C26 C25 1.414(4) . ?
C17 H17 0.9500 . ?
C6 H6 0.9500 . ?
C6 C1 1.374(4) . ?
C29 H29 1.0000 . ?
C29 C31 1.537(4) . ?
C29 C30 1.511(4) . ?
C28 H28 0.9500 . ?
C2 H2A 0.9500 . ?
C2 C1 1.393(4) . ?
C25 C32 1.512(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.380(4) . ?
C1 C7 1.540(4) . ?
C57 H57 1.0000 . ?
C57 C58 1.512(4) . ?
C57 C59 1.533(5) . ?
C51 H51 1.0000 . ?
C51 C52 1.486(4) . ?
C51 C53 1.499(5) . ?
C43 H43 0.9500 . ?
C43 C42 1.375(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 1.0000 . ?
C32 C34 1.522(5) . ?
C32 C33 1.534(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C35 H35 1.0000 . ?
C35 C36 1.519(5) . ?
C35 C37 1.533(5) . ?
C42 H42 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C8 1.513(5) . ?
C7 C9 1.483(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C69 1.540(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.530(6) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.488(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 O1 H1 106(3) . . ?
C65 O3 H3 109.5 . . ?
C39 O2 H2 109.5 . . ?
C22 N1 C66 111.3(2) . . ?
C44 N1 C66 111.34(19) . . ?
C44 N1 C22 109.11(19) . . ?
C67 O4 C70 104.8(3) . . ?
C65 C64 C66 121.0(2) . . ?
C63 C64 C65 118.2(2) . . ?
C63 C64 C66 120.9(2) . . ?
O1 C21 C20 116.8(2) . . ?
O1 C21 C16 121.4(2) . . ?
C16 C21 C20 121.8(2) . . ?
O3 C65 C64 120.7(2) . . ?
O3 C65 C60 117.9(2) . . ?
C60 C65 C64 121.4(2) . . ?
C21 C20 C22 119.3(2) . . ?
C19 C20 C21 117.8(2) . . ?
C19 C20 C22 122.8(2) . . ?
C65 C60 C48 121.9(2) . . ?
C61 C60 C65 117.9(2) . . ?
C61 C60 C48 120.1(2) . . ?
O2 C39 C38 122.2(2) . . ?
O2 C39 C40 116.5(2) . . ?
C38 C39 C40 121.3(2) . . ?
C64 C63 H63 119.2 . . ?
C62 C63 C64 121.6(2) . . ?
C62 C63 H63 119.2 . . ?
C5 C4 C16 120.3(2) . . ?
C5 C4 C3 120.0(2) . . ?
C3 C4 C16 119.7(2) . . ?
N1 C66 C64 112.04(19) . . ?
N1 C66 H66A 109.2 . . ?
N1 C66 H66B 109.2 . . ?
C64 C66 H66A 109.2 . . ?
C64 C66 H66B 109.2 . . ?
H66A C66 H66B 107.9 . . ?
C21 C16 C4 119.9(2) . . ?
C17 C16 C21 118.2(2) . . ?
C17 C16 C4 122.0(2) . . ?
C47 C48 C60 120.2(2) . . ?
C47 C48 C49 119.4(2) . . ?
C49 C48 C60 120.2(2) . . ?
C60 C61 H61 119.1 . . ?
C62 C61 C60 121.7(3) . . ?
C62 C61 H61 119.1 . . ?
N1 C22 C20 113.5(2) . . ?
N1 C22 H22A 108.9 . . ?
N1 C22 H22B 108.9 . . ?
C20 C22 H22A 108.9 . . ?
C20 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C63 C62 C61 119.1(3) . . ?
C63 C62 H62 120.4 . . ?
C61 C62 H62 120.4 . . ?
C39 C38 C26 121.4(2) . . ?
C39 C38 C43 118.3(3) . . ?
C43 C38 C26 120.2(2) . . ?
C46 C45 C51 121.7(2) . . ?
C50 C45 C46 117.3(2) . . ?
C50 C45 C51 121.0(2) . . ?
C4 C5 C13 121.3(2) . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 C13 119.2(2) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 C20 121.4(2) . . ?
C18 C19 H19 119.3 . . ?
C4 C3 C10 121.1(2) . . ?
C2 C3 C4 118.1(3) . . ?
C2 C3 C10 120.8(2) . . ?
C48 C47 C54 122.4(2) . . ?
C46 C47 C48 119.2(2) . . ?
C46 C47 C54 118.3(2) . . ?
C39 C40 C44 122.0(2) . . ?
C41 C40 C39 118.1(3) . . ?
C41 C40 C44 119.8(2) . . ?
C24 C23 C29 120.4(3) . . ?
C24 C23 C28 118.0(3) . . ?
C28 C23 C29 121.7(3) . . ?
C5 C13 H13 107.4 . . ?
C14 C13 C5 110.0(2) . . ?
C14 C13 H13 107.4 . . ?
C14 C13 C15 111.3(3) . . ?
C15 C13 C5 113.1(2) . . ?
C15 C13 H13 107.4 . . ?
C45 C46 H46 118.8 . . ?
C47 C46 C45 122.4(2) . . ?
C47 C46 H46 118.8 . . ?
C26 C27 C35 121.4(2) . . ?
C28 C27 C26 119.1(3) . . ?
C28 C27 C35 119.4(3) . . ?
C48 C49 C57 122.9(2) . . ?
C50 C49 C48 119.1(2) . . ?
C50 C49 C57 118.0(2) . . ?
N1 C44 C40 116.6(2) . . ?
N1 C44 H44A 108.1 . . ?
N1 C44 H44B 108.1 . . ?
C40 C44 H44A 108.1 . . ?
C40 C44 H44B 108.1 . . ?
H44A C44 H44B 107.3 . . ?
C3 C10 H10 107.0 . . ?
C3 C10 C12 112.7(2) . . ?
C12 C10 H10 107.0 . . ?
C11 C10 C3 112.7(2) . . ?
C11 C10 H10 107.0 . . ?
C11 C10 C12 110.1(3) . . ?
C47 C54 H54 108.4 . . ?
C56 C54 C47 110.2(2) . . ?
C56 C54 H54 108.4 . . ?
C56 C54 C55 109.9(2) . . ?
C55 C54 C47 111.6(2) . . ?
C55 C54 H54 108.4 . . ?
C45 C50 C49 122.5(2) . . ?
C45 C50 H50 118.7 . . ?
C49 C50 H50 118.7 . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.5(3) . . ?
C17 C18 H18 120.2 . . ?
C23 C24 H24 118.6 . . ?
C23 C24 C25 122.9(3) . . ?
C25 C24 H24 118.6 . . ?
C27 C26 C38 121.8(2) . . ?
C27 C26 C25 119.7(3) . . ?
C25 C26 C38 118.4(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.3(2) . . ?
C18 C17 H17 119.4 . . ?
C5 C6 H6 119.0 . . ?
C1 C6 C5 122.1(3) . . ?
C1 C6 H6 119.0 . . ?
C23 C29 H29 108.1 . . ?
C23 C29 C31 109.5(2) . . ?
C31 C29 H29 108.1 . . ?
C30 C29 C23 111.8(2) . . ?
C30 C29 H29 108.1 . . ?
C30 C29 C31 111.2(2) . . ?
C23 C28 C27 121.7(3) . . ?
C23 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C3 C2 H2A 118.8 . . ?
C1 C2 C3 122.5(3) . . ?
C1 C2 H2A 118.8 . . ?
C24 C25 C26 118.5(3) . . ?
C24 C25 C32 119.8(3) . . ?
C26 C25 C32 121.7(3) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 C40 121.4(3) . . ?
C42 C41 H41 119.3 . . ?
C6 C1 C2 118.0(3) . . ?
C6 C1 C7 121.0(3) . . ?
C2 C1 C7 121.0(3) . . ?
C49 C57 H57 108.0 . . ?
C49 C57 C59 111.9(3) . . ?
C58 C57 C49 110.8(2) . . ?
C58 C57 H57 108.0 . . ?
C58 C57 C59 110.2(2) . . ?
C59 C57 H57 108.0 . . ?
C45 C51 H51 107.3 . . ?
C52 C51 C45 112.9(2) . . ?
C52 C51 H51 107.3 . . ?
C52 C51 C53 111.2(3) . . ?
C53 C51 C45 110.6(3) . . ?
C53 C51 H51 107.3 . . ?
C38 C43 H43 119.2 . . ?
C42 C43 C38 121.6(3) . . ?
C42 C43 H43 119.2 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C32 H32 108.2 . . ?
C25 C32 C34 111.2(3) . . ?
C25 C32 C33 111.2(3) . . ?
C34 C32 H32 108.2 . . ?
C34 C32 C33 109.7(3) . . ?
C33 C32 H32 108.2 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C27 C35 H35 107.7 . . ?
C27 C35 C36 112.0(2) . . ?
C27 C35 C37 110.1(3) . . ?
C36 C35 H35 107.7 . . ?
C36 C35 C37 111.5(3) . . ?
C37 C35 H35 107.7 . . ?
C41 C42 H42 120.4 . . ?
C43 C42 C41 119.2(3) . . ?
C43 C42 H42 120.4 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 C7 H7 107.3 . . ?
C8 C7 C1 111.4(2) . . ?
C8 C7 H7 107.3 . . ?
C9 C7 C1 111.9(3) . . ?
C9 C7 H7 107.3 . . ?
C9 C7 C8 111.3(3) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C70 H70A 110.4 . . ?
O4 C70 H70B 110.4 . . ?
O4 C70 C69 106.5(3) . . ?
H70A C70 H70B 108.6 . . ?
C69 C70 H70A 110.4 . . ?
C69 C70 H70B 110.4 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C67 H67A 110.9 . . ?
O4 C67 H67B 110.9 . . ?
O4 C67 C68 104.1(4) . . ?
H67A C67 H67B 108.9 . . ?
C68 C67 H67A 110.9 . . ?
C68 C67 H67B 110.9 . . ?
C67 C68 H68A 110.8 . . ?
C67 C68 H68B 110.8 . . ?
H68A C68 H68B 108.9 . . ?
C69 C68 C67 104.5(4) . . ?
C69 C68 H68A 110.8 . . ?
C69 C68 H68B 110.8 . . ?
C70 C69 H69A 111.1 . . ?
C70 C69 H69B 111.1 . . ?
C68 C69 C70 103.1(4) . . ?
C68 C69 H69A 111.1 . . ?
C68 C69 H69B 111.1 . . ?
H69A C69 H69B 109.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pbca
_database_code_depnum_ccdc_archive 'CCDC 1894390'
loop_
_audit_author_name
_audit_author_address
'Dae Young Bae'
;Pohang University of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-17 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
_audit_creation_date             2019-02-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C75 H99.05 Mn N Na2 O6'
_chemical_formula_sum            'C75 H99.06 Mn N Na2 O6'
_chemical_formula_weight         1211.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.612(4)
_cell_length_b                   27.311(6)
_cell_length_c                   30.616(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15562(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    60522
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.482
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            60522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.482
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7000
_diffrn_source                   'PLSII 2D bending magnet'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9297
_reflns_number_total             15909
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         15909
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0682
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1331P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2275
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 C73, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C73, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C29A, C30, C31A, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=1-FVAR(1)
 Sof(H10)=Sof(H10A)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H57(0.5) H57A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C29(0.5) H29(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C29A(0.5) H29A(0.5) C31A(0.5) H31D(0.5)
 H31E(0.5) H31F(0.5) C58A(0.5) H58D(0.5) H58E(0.5) H58F(0.5)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C35(H35), C7(H7), C54(H54), C57(H57), C57(H57A), C10(H10),
 C10(H10A), C32(H32), C29(H29), C29A(H29A)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C44(H44A,H44B), C66(H66A,H66B), C75(H75A,H75B), C72(H72A,
 H72B), C73(H73A,H73B), C74(H74A,H74B)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C6(H6), C17(H17), C18(H18), C41(H41), C40(H40), C50(H50), C69(H69),
 C46(H46), C2(H2), C63(H63), C65(H65), C39(H39), C64(H64), C28(H28), C24(H24)
4.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C15(H15A,H15B,H15C), C67(H67A,H67B,H67C), C14(H14A,H14B,
 H14C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C52(H52A,
 H52B,H52C), C8(H8A,H8B,H8C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C9(H9A,
 H9B,H9C), C30(H30D,H30E,H30F), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C),
 C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C58(H58A,H58B,H58C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C31A(H31D,H31E,H31F), C58A(H58D,H58E,H58F),
 C53(H53A,H53B,H53C), C12A(H12D,H12E,H12F), C11A(H11D,H11E,H11F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.66264(2) 0.30556(2) 0.64459(2) 0.05038(15) Uani 1 1 d . . . . .
Na1 Na 0.73621(6) 0.21244(5) 0.58897(4) 0.0642(3) Uani 1 1 d . . . . .
Na2 Na 0.80974(7) 0.33179(5) 0.58751(4) 0.0654(3) Uani 1 1 d . . . . .
O3 O 0.69977(10) 0.36055(7) 0.60278(6) 0.0524(5) Uani 1 1 d . . . . .
O1 O 0.62515(10) 0.24649(7) 0.60748(6) 0.0514(5) Uani 1 1 d . . . . .
O4 O 0.76817(10) 0.27435(8) 0.63952(6) 0.0546(5) Uani 1 1 d . . . . .
O2 O 0.65803(10) 0.31089(9) 0.70989(7) 0.0628(6) Uani 1 1 d . . . . .
O5 O 0.85203(11) 0.25294(9) 0.56800(7) 0.0644(6) Uani 1 1 d . . . . .
N1 N 0.55411(12) 0.34054(9) 0.64051(7) 0.0484(6) Uani 1 1 d . . . . .
C5 C 0.66651(15) 0.20659(12) 0.50178(10) 0.0539(7) Uani 1 1 d . . . . .
C61 C 0.67085(15) 0.40410(12) 0.59541(10) 0.0539(7) Uani 1 1 d . . . . .
C19 C 0.43581(15) 0.26436(12) 0.57947(10) 0.0558(8) Uani 1 1 d . . . . .
H19 H 0.3947 0.2812 0.5900 0.067 Uiso 1 1 calc R . . . .
C4 C 0.61845(15) 0.18580(11) 0.53269(10) 0.0525(7) Uani 1 1 d . . . . .
C13 C 0.65401(16) 0.25664(13) 0.48273(10) 0.0601(8) Uani 1 1 d . . . . .
H13 H 0.6015 0.2638 0.4853 0.072 Uiso 1 1 calc R . . . .
C16 C 0.55529(15) 0.21451(11) 0.54881(9) 0.0495(7) Uani 1 1 d . . . . .
C20 C 0.50006(14) 0.26844(11) 0.60223(9) 0.0496(7) Uani 1 1 d . . . . .
O6 O 0.78002(15) 0.15012(11) 0.63397(10) 0.0922(8) Uani 1 1 d . . . . .
C70 C 0.89854(16) 0.24367(12) 0.59582(11) 0.0570(8) Uani 1 1 d . . . . .
C6 C 0.72808(16) 0.17915(13) 0.49007(11) 0.0597(8) Uani 1 1 d . . . . .
H6 H 0.7615 0.1930 0.4701 0.072 Uiso 1 1 calc R . . . .
C17 C 0.48971(16) 0.21184(12) 0.52721(10) 0.0552(7) Uani 1 1 d . . . . .
H17 H 0.4861 0.1924 0.5016 0.066 Uiso 1 1 calc R . . . .
C22 C 0.50242(15) 0.29929(11) 0.64303(10) 0.0522(7) Uani 1 1 d . . . . .
H22A H 0.4538 0.3126 0.6487 0.063 Uiso 1 1 calc R . . . .
H22B H 0.5155 0.2782 0.6681 0.063 Uiso 1 1 calc R . . . .
C62 C 0.59487(16) 0.41082(12) 0.59396(10) 0.0558(7) Uani 1 1 d . . . . .
C18 C 0.42983(16) 0.23654(12) 0.54188(10) 0.0580(8) Uani 1 1 d . . . . .
H18 H 0.3855 0.2345 0.5266 0.070 Uiso 1 1 calc R . . . .
C41 C 0.48858(16) 0.35927(13) 0.75080(11) 0.0611(8) Uani 1 1 d . . . . .
H41 H 0.4499 0.3794 0.7415 0.073 Uiso 1 1 calc R . . . .
C44 C 0.54474(16) 0.37436(12) 0.67814(10) 0.0558(7) Uani 1 1 d . . . . .
H44A H 0.4989 0.3922 0.6743 0.067 Uiso 1 1 calc R . . . .
H44B H 0.5840 0.3988 0.6775 0.067 Uiso 1 1 calc R . . . .
C66 C 0.54494(14) 0.36834(11) 0.59868(10) 0.0536(7) Uani 1 1 d . . . . .
H66A H 0.5526 0.3457 0.5739 0.064 Uiso 1 1 calc R . . . .
H66B H 0.4949 0.3804 0.5969 0.064 Uiso 1 1 calc R . . . .
C27 C 0.72444(16) 0.28350(15) 0.80945(10) 0.0660(9) Uani 1 1 d . . . . .
C1 C 0.74144(17) 0.13300(13) 0.50649(11) 0.0603(8) Uani 1 1 d . . . . .
C42 C 0.54434(15) 0.35025(12) 0.72256(10) 0.0571(8) Uani 1 1 d . . . . .
C40 C 0.48746(17) 0.33961(14) 0.79255(11) 0.0672(9) Uani 1 1 d . . . . .
H40 H 0.4489 0.3465 0.8119 0.081 Uiso 1 1 calc R . . . .
C21 C 0.56204(14) 0.24325(11) 0.58710(10) 0.0499(7) Uani 1 1 d . . . . .
C26 C 0.65916(16) 0.26518(15) 0.79248(11) 0.0676(9) Uani 1 1 d . . . . .
C35 C 0.73631(16) 0.33805(15) 0.81255(11) 0.0675(9) Uani 1 1 d . . . . .
H35 H 0.7138 0.3531 0.7861 0.081 Uiso 1 1 calc R . . . .
C60 C 0.71538(16) 0.44500(12) 0.58823(12) 0.0626(8) Uani 1 1 d . . . . .
C48 C 0.79549(16) 0.43795(12) 0.59056(12) 0.0616(8) Uani 1 1 d . . . . .
C50 C 0.90451(17) 0.43189(13) 0.63269(11) 0.0632(8) Uani 1 1 d . . . . .
H50 H 0.9283 0.4338 0.6601 0.076 Uiso 1 1 calc R . . . .
C3 C 0.63118(17) 0.13811(13) 0.54856(11) 0.0623(8) Uani 1 1 d . . . . .
C69 C 0.88899(16) 0.25050(14) 0.64110(11) 0.0644(9) Uani 1 1 d . . . . .
H69 H 0.9295 0.2451 0.6593 0.077 Uiso 1 1 calc R . . . .
C46 C 0.90827(17) 0.41839(13) 0.55618(11) 0.0657(9) Uani 1 1 d . . . . .
H46 H 0.9348 0.4110 0.5305 0.079 Uiso 1 1 calc R . . . .
C2 C 0.69216(17) 0.11259(13) 0.53506(11) 0.0652(8) Uani 1 1 d . . . . .
H2 H 0.7001 0.0804 0.5457 0.078 Uiso 1 1 calc R . . . .
C63 C 0.56721(18) 0.45651(13) 0.58570(12) 0.0713(10) Uani 1 1 d . . . . .
H63 H 0.5166 0.4607 0.5848 0.086 Uiso 1 1 calc R . . . .
C45 C 0.94425(16) 0.42067(13) 0.59569(11) 0.0637(8) Uani 1 1 d . . . . .
C43 C 0.60311(15) 0.31999(13) 0.73566(10) 0.0574(8) Uani 1 1 d . . . . .
C49 C 0.83068(17) 0.44050(13) 0.63086(12) 0.0637(8) Uani 1 1 d . . . . .
C51 C 1.02528(17) 0.41169(15) 0.59915(12) 0.0691(9) Uani 1 1 d . . . . .
C71 C 0.97022(17) 0.22454(14) 0.58034(12) 0.0695(9) Uani 1 1 d . . . . .
H71A H 0.9749 0.2302 0.5489 0.104 Uiso 1 1 calc GR . . . .
H71B H 0.9734 0.1894 0.5863 0.104 Uiso 1 1 calc GR . . . .
H71C H 1.0089 0.2416 0.5958 0.104 Uiso 1 1 calc GR . . . .
C47 C 0.83483(16) 0.42654(13) 0.55259(11) 0.0633(9) Uani 1 1 d . . . . .
C38 C 0.60071(16) 0.29966(13) 0.77830(11) 0.0626(8) Uani 1 1 d . . . . .
C65 C 0.6856(2) 0.49011(14) 0.58025(15) 0.0825(11) Uani 1 1 d . . . . .
H65 H 0.7164 0.5174 0.5757 0.099 Uiso 1 1 calc R . . . .
C15 C 0.6941(2) 0.29554(14) 0.50894(13) 0.0756(10) Uani 1 1 d . . . . .
H15A H 0.6765 0.2956 0.5391 0.113 Uiso 1 1 calc GR . . . .
H15B H 0.6859 0.3278 0.4958 0.113 Uiso 1 1 calc GR . . . .
H15C H 0.7456 0.2882 0.5088 0.113 Uiso 1 1 calc GR . . . .
C39 C 0.54343(17) 0.30995(15) 0.80534(11) 0.0689(9) Uani 1 1 d . . . . .
H39 H 0.5426 0.2961 0.8338 0.083 Uiso 1 1 calc R . . . .
C67 C 0.82193(19) 0.26836(15) 0.71038(11) 0.0716(10) Uani 1 1 d . . . . .
H67A H 0.8122 0.3024 0.7187 0.107 Uiso 1 1 calc GR . . . .
H67B H 0.8678 0.2580 0.7230 0.107 Uiso 1 1 calc GR . . . .
H67C H 0.7833 0.2473 0.7214 0.107 Uiso 1 1 calc GR . . . .
C64 C 0.6114(2) 0.49701(15) 0.57862(16) 0.0883(13) Uani 1 1 d . . . . .
H64 H 0.5915 0.5284 0.5728 0.106 Uiso 1 1 calc R . . . .
C7 C 0.80836(18) 0.10391(14) 0.49294(12) 0.0689(9) Uani 1 1 d . . . . .
H7 H 0.8092 0.0735 0.5111 0.083 Uiso 1 1 calc R . . . .
C54 C 0.79838(19) 0.42333(15) 0.50787(12) 0.0748(10) Uani 1 1 d . . . . .
H54 H 0.7466 0.4152 0.5127 0.090 Uiso 1 1 calc R . . . .
C68 C 0.82553(16) 0.26446(12) 0.66130(11) 0.0572(8) Uani 1 1 d . . . . .
C14 C 0.6741(2) 0.26058(15) 0.43424(12) 0.0768(10) Uani 1 1 d . . . . .
H14A H 0.7263 0.2572 0.4310 0.115 Uiso 1 1 calc GR . . . .
H14B H 0.6590 0.2925 0.4230 0.115 Uiso 1 1 calc GR . . . .
H14C H 0.6500 0.2345 0.4178 0.115 Uiso 1 1 calc GR . . . .
C37 C 0.6982(2) 0.36052(19) 0.85308(13) 0.0910(13) Uani 1 1 d . . . . .
H37A H 0.6463 0.3550 0.8509 0.136 Uiso 1 1 calc GR . . . .
H37B H 0.7078 0.3958 0.8542 0.136 Uiso 1 1 calc GR . . . .
H37C H 0.7166 0.3450 0.8797 0.136 Uiso 1 1 calc GR . . . .
C28 C 0.77604(18) 0.25084(17) 0.82363(12) 0.0787(11) Uani 1 1 d . . . . .
H28 H 0.8194 0.2632 0.8358 0.094 Uiso 1 1 calc R . . . .
C36 C 0.81499(17) 0.35381(16) 0.81293(12) 0.0753(10) Uani 1 1 d . . . . .
H36A H 0.8368 0.3448 0.8409 0.113 Uiso 1 1 calc GR . . . .
H36B H 0.8180 0.3894 0.8089 0.113 Uiso 1 1 calc GR . . . .
H36C H 0.8407 0.3374 0.7892 0.113 Uiso 1 1 calc GR . . . .
C57 C 0.7900(2) 0.45272(16) 0.67288(12) 0.0768(10) Uani 1 1 d . . . . .
H57 H 0.7396 0.4628 0.6661 0.092 Uiso 0.5 1 calc R . P A 1
H57A H 0.7391 0.4520 0.6626 0.092 Uiso 0.5 1 calc R . P B 2
C25 C 0.64852(19) 0.21463(17) 0.78999(15) 0.0837(11) Uani 1 1 d . . . . .
C56 C 0.8300(2) 0.38414(17) 0.47845(13) 0.0844(11) Uani 1 1 d . . . . .
H56A H 0.8780 0.3942 0.4689 0.127 Uiso 1 1 calc GR . . . .
H56B H 0.7990 0.3797 0.4529 0.127 Uiso 1 1 calc GR . . . .
H56C H 0.8333 0.3532 0.4946 0.127 Uiso 1 1 calc GR . . . .
C52 C 1.0657(2) 0.45742(19) 0.58626(17) 0.1079(16) Uani 1 1 d . . . . .
H52A H 1.0547 0.4656 0.5558 0.162 Uiso 1 1 calc GR . . . .
H52B H 1.1174 0.4518 0.5894 0.162 Uiso 1 1 calc GR . . . .
H52C H 1.0511 0.4846 0.6052 0.162 Uiso 1 1 calc GR . . . .
C8 C 0.87789(19) 0.13195(17) 0.50267(17) 0.0960(13) Uani 1 1 d . . . . .
H8A H 0.8806 0.1609 0.4839 0.144 Uiso 1 1 calc GR . . . .
H8B H 0.9193 0.1107 0.4970 0.144 Uiso 1 1 calc GR . . . .
H8C H 0.8782 0.1421 0.5334 0.144 Uiso 1 1 calc GR . . . .
C55 C 0.8019(3) 0.47301(17) 0.48564(17) 0.1138(17) Uani 1 1 d . . . . .
H55A H 0.7778 0.4975 0.5039 0.171 Uiso 1 1 calc GR . . . .
H55B H 0.7779 0.4712 0.4572 0.171 Uiso 1 1 calc GR . . . .
H55C H 0.8523 0.4824 0.4815 0.171 Uiso 1 1 calc GR . . . .
C10 C 0.5779(2) 0.11372(14) 0.57949(15) 0.0829(12) Uani 1 1 d . . . . .
H10 H 0.5554 0.1416 0.5957 0.099 Uiso 0.527(11) 1 calc R . P C 1
H10A H 0.5324 0.1326 0.5752 0.099 Uiso 0.527(11) 1 calc R . P C 2
C59 C 0.7906(3) 0.41169(17) 0.70492(14) 0.0990(14) Uani 1 1 d . . . . .
H59A H 0.7772 0.3812 0.6901 0.149 Uiso 1 1 calc GR . . . .
H59B H 0.7561 0.4186 0.7283 0.149 Uiso 1 1 calc GR . . . .
H59C H 0.8388 0.4083 0.7174 0.149 Uiso 1 1 calc GR . . . .
C9 C 0.8055(2) 0.08823(17) 0.44657(13) 0.0914(12) Uani 1 1 d . . . . .
H9A H 0.7593 0.0723 0.4408 0.137 Uiso 1 1 calc GR . . . .
H9B H 0.8446 0.0652 0.4407 0.137 Uiso 1 1 calc GR . . . .
H9C H 0.8106 0.1169 0.4276 0.137 Uiso 1 1 calc GR . . . .
C30 C 0.8965(2) 0.17503(18) 0.81570(16) 0.0965(13) Uani 1 1 d . U . . .
H30D H 0.8866 0.1579 0.7882 0.145 Uiso 0.5 1 calc GR . P D 2
H30E H 0.9374 0.1595 0.8304 0.145 Uiso 0.5 1 calc GR . P D 2
H30F H 0.9079 0.2094 0.8096 0.145 Uiso 0.5 1 calc GR . P D 2
H30A H 0.8999 0.1836 0.7847 0.145 Uiso 0.5 1 calc GR . P E 1
H30B H 0.9309 0.1489 0.8223 0.145 Uiso 0.5 1 calc GR . P E 1
H30C H 0.9076 0.2039 0.8335 0.145 Uiso 0.5 1 calc GR . P E 1
C24 C 0.7024(2) 0.18399(17) 0.80398(18) 0.1003(15) Uani 1 1 d . . . . .
H24 H 0.6948 0.1497 0.8019 0.120 Uiso 1 1 calc R . . . .
C32 C 0.5793(2) 0.19397(17) 0.77076(19) 0.0988(14) Uani 1 1 d . . . . .
H32 H 0.5453 0.2221 0.7677 0.119 Uiso 1 1 calc R . . . .
C23 C 0.7665(2) 0.20025(19) 0.82071(17) 0.1006(15) Uani 1 1 d . . . . .
C75 C 0.8394(2) 0.11815(19) 0.6245(2) 0.1103(16) Uani 1 1 d . . . . .
H75A H 0.8810 0.1377 0.6145 0.132 Uiso 1 1 calc R . . . .
H75B H 0.8259 0.0953 0.6008 0.132 Uiso 1 1 calc R . . . .
C34 C 0.5438(3) 0.1577(2) 0.8010(2) 0.1258(19) Uani 1 1 d . . . . .
H34A H 0.5733 0.1280 0.8029 0.189 Uiso 1 1 calc GR . . . .
H34B H 0.4961 0.1493 0.7897 0.189 Uiso 1 1 calc GR . . . .
H34C H 0.5389 0.1722 0.8302 0.189 Uiso 1 1 calc GR . . . .
C33 C 0.5925(3) 0.1752(3) 0.7264(2) 0.146(2) Uani 1 1 d . . . . .
H33A H 0.6217 0.1988 0.7101 0.218 Uiso 1 1 calc GR . . . .
H33B H 0.5465 0.1704 0.7114 0.218 Uiso 1 1 calc GR . . . .
H33C H 0.6180 0.1439 0.7282 0.218 Uiso 1 1 calc GR . . . .
C29 C 0.8252(5) 0.1721(4) 0.8475(4) 0.072(2) Uani 0.5 1 d . U P F 2
H29 H 0.8339 0.1872 0.8768 0.087 Uiso 0.5 1 calc R . P F 2
C72 C 0.7660(4) 0.1447(3) 0.67853(18) 0.134(2) Uani 1 1 d . U . . .
H72A H 0.7237 0.1233 0.6830 0.161 Uiso 1 1 calc R . . . .
H72B H 0.7561 0.1770 0.6920 0.161 Uiso 1 1 calc R . . . .
C73 C 0.8299(4) 0.1226(3) 0.6982(2) 0.148(2) Uani 1 1 d . U . . .
H73A H 0.8171 0.1033 0.7244 0.178 Uiso 1 1 calc R . . . .
H73B H 0.8653 0.1481 0.7065 0.178 Uiso 1 1 calc R . . . .
C74 C 0.8587(4) 0.0907(3) 0.6634(2) 0.152(3) Uani 1 1 d . U . . .
H74A H 0.9115 0.0868 0.6659 0.183 Uiso 1 1 calc R . . . .
H74B H 0.8357 0.0580 0.6637 0.183 Uiso 1 1 calc R . . . .
C31 C 0.8031(5) 0.1177(3) 0.8510(3) 0.085(2) Uani 0.5 1 d . U P F 2
H31A H 0.7936 0.1047 0.8217 0.128 Uiso 0.5 1 calc GR . P F 2
H31B H 0.7596 0.1149 0.8688 0.128 Uiso 0.5 1 calc GR . P F 2
H31C H 0.8420 0.0989 0.8645 0.128 Uiso 0.5 1 calc GR . P F 2
C58 C 0.8303(7) 0.4946(4) 0.7017(4) 0.093(3) Uani 0.5 1 d . . P G 1
H58A H 0.8659 0.4791 0.7209 0.139 Uiso 0.5 1 calc GR . P G 1
H58B H 0.7948 0.5121 0.7194 0.139 Uiso 0.5 1 calc GR . P G 1
H58C H 0.8545 0.5177 0.6821 0.139 Uiso 0.5 1 calc GR . P G 1
C11 C 0.6217(5) 0.0816(4) 0.6183(3) 0.102(4) Uani 0.527(11) 1 d . . P C 1
H11A H 0.6382 0.0504 0.6061 0.153 Uiso 0.527(11) 1 calc GR . P C 1
H11B H 0.5892 0.0752 0.6428 0.153 Uiso 0.527(11) 1 calc GR . P C 1
H11C H 0.6632 0.1004 0.6286 0.153 Uiso 0.527(11) 1 calc GR . P C 1
C12 C 0.5590(6) 0.0593(4) 0.5617(3) 0.083(3) Uani 0.527(11) 1 d . . P C 2
H12A H 0.5470 0.0610 0.5306 0.125 Uiso 0.527(11) 1 calc GR . P C 2
H12B H 0.5180 0.0462 0.5780 0.125 Uiso 0.527(11) 1 calc GR . P C 2
H12C H 0.6007 0.0378 0.5658 0.125 Uiso 0.527(11) 1 calc GR . P C 2
C29A C 0.8254(5) 0.1586(4) 0.8253(4) 0.086(3) Uani 0.5 1 d . U P F 1
H29A H 0.8125 0.1293 0.8073 0.103 Uiso 0.5 1 calc R . P F 1
C31A C 0.8243(6) 0.1469(5) 0.8715(4) 0.104(3) Uani 0.5 1 d . U P F 1
H31D H 0.8610 0.1222 0.8778 0.156 Uiso 0.5 1 calc GR . P F 1
H31E H 0.7769 0.1342 0.8795 0.156 Uiso 0.5 1 calc GR . P F 1
H31F H 0.8344 0.1766 0.8885 0.156 Uiso 0.5 1 calc GR . P F 1
C58A C 0.8000(10) 0.5029(6) 0.6806(5) 0.135(6) Uani 0.5 1 d . . P G 2
H58D H 0.8472 0.5082 0.6939 0.203 Uiso 0.5 1 calc GR . P G 2
H58E H 0.7625 0.5148 0.7003 0.203 Uiso 0.5 1 calc GR . P G 2
H58F H 0.7974 0.5207 0.6528 0.203 Uiso 0.5 1 calc GR . P G 2
C53 C 1.0486(2) 0.36904(19) 0.57200(14) 0.0995(15) Uani 1 1 d . . . . .
H53A H 1.0243 0.3393 0.5822 0.149 Uiso 1 1 calc GR . . . .
H53B H 1.1007 0.3648 0.5747 0.149 Uiso 1 1 calc GR . . . .
H53C H 1.0362 0.3750 0.5414 0.149 Uiso 1 1 calc GR . . . .
C12A C 0.5228(6) 0.0898(4) 0.5619(3) 0.085(3) Uani 0.473(11) 1 d . . P C 1
H12D H 0.4914 0.1131 0.5467 0.128 Uiso 0.473(11) 1 calc GR . P C 1
H12E H 0.4955 0.0733 0.5850 0.128 Uiso 0.473(11) 1 calc GR . P C 1
H12F H 0.5407 0.0655 0.5410 0.128 Uiso 0.473(11) 1 calc GR . P C 1
C11A C 0.5910(5) 0.1173(4) 0.6223(3) 0.070(3) Uani 0.473(11) 1 d . . P C 2
H11D H 0.6370 0.1015 0.6290 0.106 Uiso 0.473(11) 1 calc GR . P C 2
H11E H 0.5524 0.1011 0.6386 0.106 Uiso 0.473(11) 1 calc GR . P C 2
H11F H 0.5932 0.1519 0.6306 0.106 Uiso 0.473(11) 1 calc GR . P C 2
H51 H 1.0384(16) 0.4016(11) 0.6320(10) 0.056(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.091(2) . ?
Mn1 O1 2.093(2) . ?
Mn1 O4 2.1467(19) . ?
Mn1 O2 2.006(2) . ?
Mn1 N1 2.238(2) . ?
Na1 O1 2.336(2) . ?
Na1 O4 2.368(2) . ?
Na1 O5 2.507(3) . ?
Na1 C5 2.972(3) . ?
Na1 C4 2.881(3) . ?
Na1 O6 2.337(3) . ?
Na1 C3 3.078(4) . ?
Na2 O3 2.242(2) . ?
Na2 O4 2.365(2) . ?
Na2 O5 2.369(3) . ?
Na2 C48 2.913(4) . ?
Na2 C47 2.838(4) . ?
O3 C61 1.325(4) . ?
O1 C21 1.333(3) . ?
O4 C68 1.287(3) . ?
O2 C43 1.315(4) . ?
O5 C70 1.240(4) . ?
N1 C22 1.483(4) . ?
N1 C44 1.487(4) . ?
N1 C66 1.498(4) . ?
C5 C4 1.421(4) . ?
C5 C13 1.504(5) . ?
C5 C6 1.415(4) . ?
C61 C62 1.427(4) . ?
C61 C60 1.408(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.388(4) . ?
C19 C18 1.383(4) . ?
C4 C16 1.497(4) . ?
C4 C3 1.410(5) . ?
C13 H13 1.0000 . ?
C13 C15 1.526(5) . ?
C13 C14 1.535(5) . ?
C16 C17 1.390(4) . ?
C16 C21 1.416(4) . ?
C20 C22 1.507(4) . ?
C20 C21 1.421(4) . ?
O6 C75 1.437(5) . ?
O6 C72 1.397(6) . ?
C70 C69 1.410(5) . ?
C70 C71 1.509(4) . ?
C6 H6 0.9500 . ?
C6 C1 1.379(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C62 C66 1.493(4) . ?
C62 C63 1.374(5) . ?
C18 H18 0.9500 . ?
C41 H41 0.9500 . ?
C41 C42 1.373(4) . ?
C41 C40 1.387(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C42 1.511(4) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C27 C26 1.413(5) . ?
C27 C35 1.509(5) . ?
C27 C28 1.381(5) . ?
C1 C2 1.385(5) . ?
C1 C7 1.534(4) . ?
C42 C43 1.428(4) . ?
C40 H40 0.9500 . ?
C40 C39 1.376(5) . ?
C26 C38 1.503(5) . ?
C26 C25 1.397(6) . ?
C35 H35 1.0000 . ?
C35 C37 1.555(5) . ?
C35 C36 1.526(5) . ?
C60 C48 1.505(4) . ?
C60 C65 1.373(5) . ?
C48 C49 1.399(5) . ?
C48 C47 1.409(5) . ?
C50 H50 0.9500 . ?
C50 C45 1.387(5) . ?
C50 C49 1.395(4) . ?
C3 C2 1.395(4) . ?
C3 C10 1.524(5) . ?
C69 H69 0.9500 . ?
C69 C68 1.387(4) . ?
C46 H46 0.9500 . ?
C46 C45 1.384(5) . ?
C46 C47 1.389(4) . ?
C2 H2 0.9500 . ?
C63 H63 0.9500 . ?
C63 C64 1.395(5) . ?
C45 C51 1.532(4) . ?
C43 C38 1.419(5) . ?
C49 C57 1.529(5) . ?
C51 C52 1.510(6) . ?
C51 C53 1.496(5) . ?
C51 H51 1.07(3) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C47 C54 1.531(5) . ?
C38 C39 1.379(4) . ?
C65 H65 0.9500 . ?
C65 C64 1.395(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C39 H39 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C67 C68 1.508(5) . ?
C64 H64 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.533(5) . ?
C7 C9 1.484(5) . ?
C54 H54 1.0000 . ?
C54 C56 1.517(6) . ?
C54 C55 1.519(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C28 H28 0.9500 . ?
C28 C23 1.396(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C57 H57 1.0000 . ?
C57 H57A 1.0000 . ?
C57 C59 1.489(6) . ?
C57 C58 1.626(12) . ?
C57 C58A 1.403(16) . ?
C25 C24 1.374(6) . ?
C25 C32 1.525(6) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C10 H10 1.0000 . ?
C10 H10A 1.0000 . ?
C10 C11 1.688(10) . ?
C10 C12 1.621(10) . ?
C10 C12A 1.330(9) . ?
C10 C11A 1.335(8) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C30 H30D 0.9800 . ?
C30 H30E 0.9800 . ?
C30 H30F 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C30 C29 1.649(11) . ?
C30 C29A 1.429(11) . ?
C24 H24 0.9500 . ?
C24 C23 1.372(6) . ?
C32 H32 1.0000 . ?
C32 C34 1.510(7) . ?
C32 C33 1.472(8) . ?
C23 C29 1.569(11) . ?
C23 C29A 1.587(12) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C74 1.451(8) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C31 1.546(15) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 C73 1.462(8) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.478(9) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C29A H29A 1.0000 . ?
C29A C31A 1.450(15) . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C58A H58D 0.9800 . ?
C58A H58E 0.9800 . ?
C58A H58F 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O1 109.36(8) . . ?
O3 Mn1 O4 86.47(8) . . ?
O3 Mn1 N1 87.57(8) . . ?
O1 Mn1 O4 87.69(8) . . ?
O1 Mn1 N1 89.87(8) . . ?
O4 Mn1 N1 172.42(8) . . ?
O2 Mn1 O3 124.90(9) . . ?
O2 Mn1 O1 125.63(9) . . ?
O2 Mn1 O4 98.05(8) . . ?
O2 Mn1 N1 89.21(8) . . ?
O1 Na1 O4 77.26(8) . . ?
O1 Na1 O5 130.35(9) . . ?
O1 Na1 C5 81.55(8) . . ?
O1 Na1 C4 64.70(8) . . ?
O1 Na1 O6 117.11(10) . . ?
O1 Na1 C3 78.35(8) . . ?
O4 Na1 O5 68.67(8) . . ?
O4 Na1 C5 137.31(10) . . ?
O4 Na1 C4 139.66(9) . . ?
O4 Na1 C3 153.27(9) . . ?
O5 Na1 C5 99.74(9) . . ?
O5 Na1 C4 127.77(9) . . ?
O5 Na1 C3 137.25(9) . . ?
C5 Na1 C3 47.65(9) . . ?
C4 Na1 C5 28.03(8) . . ?
C4 Na1 C3 27.12(9) . . ?
O6 Na1 O4 92.70(10) . . ?
O6 Na1 O5 99.92(10) . . ?
O6 Na1 C5 129.99(11) . . ?
O6 Na1 C4 115.73(11) . . ?
O6 Na1 C3 88.75(11) . . ?
O3 Na2 O4 78.07(8) . . ?
O3 Na2 O5 132.41(9) . . ?
O3 Na2 C48 63.99(8) . . ?
O3 Na2 C47 84.80(9) . . ?
O4 Na2 O5 71.07(8) . . ?
O4 Na2 C48 127.50(10) . . ?
O4 Na2 C47 155.78(11) . . ?
O5 Na2 C48 160.56(10) . . ?
O5 Na2 C47 132.76(11) . . ?
C47 Na2 C48 28.32(10) . . ?
Mn1 O3 Na2 100.24(9) . . ?
C61 O3 Mn1 127.94(17) . . ?
C61 O3 Na2 130.54(18) . . ?
Mn1 O1 Na1 98.25(8) . . ?
C21 O1 Mn1 126.81(18) . . ?
C21 O1 Na1 129.76(18) . . ?
Mn1 O4 Na1 95.80(8) . . ?
Mn1 O4 Na2 94.86(8) . . ?
Na2 O4 Na1 96.65(9) . . ?
C68 O4 Mn1 143.6(2) . . ?
C68 O4 Na1 113.4(2) . . ?
C68 O4 Na2 102.51(18) . . ?
C43 O2 Mn1 130.15(18) . . ?
Na2 O5 Na1 92.91(8) . . ?
C70 O5 Na1 109.5(2) . . ?
C70 O5 Na2 104.1(2) . . ?
C22 N1 Mn1 104.97(17) . . ?
C22 N1 C44 110.8(2) . . ?
C22 N1 C66 110.8(2) . . ?
C44 N1 Mn1 109.12(16) . . ?
C44 N1 C66 109.5(2) . . ?
C66 N1 Mn1 111.52(16) . . ?
C4 C5 Na1 72.43(17) . . ?
C4 C5 C13 121.6(3) . . ?
C13 C5 Na1 111.5(2) . . ?
C6 C5 Na1 84.41(18) . . ?
C6 C5 C4 117.8(3) . . ?
C6 C5 C13 120.5(3) . . ?
O3 C61 C62 121.6(3) . . ?
O3 C61 C60 120.0(3) . . ?
C60 C61 C62 118.5(3) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C18 C19 C20 122.1(3) . . ?
C5 C4 Na1 79.54(17) . . ?
C5 C4 C16 120.3(3) . . ?
C16 C4 Na1 105.54(18) . . ?
C3 C4 Na1 84.22(19) . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 C16 120.1(3) . . ?
C5 C13 H13 107.4 . . ?
C5 C13 C15 110.7(3) . . ?
C5 C13 C14 113.6(3) . . ?
C15 C13 H13 107.4 . . ?
C15 C13 C14 109.9(3) . . ?
C14 C13 H13 107.4 . . ?
C17 C16 C4 120.4(3) . . ?
C17 C16 C21 120.0(3) . . ?
C21 C16 C4 119.6(2) . . ?
C19 C20 C22 119.1(3) . . ?
C19 C20 C21 119.8(3) . . ?
C21 C20 C22 121.1(3) . . ?
C75 O6 Na1 126.3(3) . . ?
C72 O6 Na1 126.0(3) . . ?
C72 O6 C75 106.0(4) . . ?
O5 C70 C69 124.1(3) . . ?
O5 C70 C71 118.2(3) . . ?
C69 C70 C71 117.8(3) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 C5 122.5(3) . . ?
C1 C6 H6 118.7 . . ?
C16 C17 H17 119.0 . . ?
C18 C17 C16 122.0(3) . . ?
C18 C17 H17 119.0 . . ?
N1 C22 C20 113.6(2) . . ?
N1 C22 H22A 108.8 . . ?
N1 C22 H22B 108.8 . . ?
C20 C22 H22A 108.8 . . ?
C20 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C61 C62 C66 120.9(3) . . ?
C63 C62 C61 119.6(3) . . ?
C63 C62 C66 119.4(3) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 C19 118.4(3) . . ?
C17 C18 H18 120.8 . . ?
C42 C41 H41 119.3 . . ?
C42 C41 C40 121.5(3) . . ?
C40 C41 H41 119.3 . . ?
N1 C44 H44A 108.4 . . ?
N1 C44 H44B 108.4 . . ?
N1 C44 C42 115.3(3) . . ?
H44A C44 H44B 107.5 . . ?
C42 C44 H44A 108.4 . . ?
C42 C44 H44B 108.4 . . ?
N1 C66 H66A 108.8 . . ?
N1 C66 H66B 108.8 . . ?
C62 C66 N1 113.9(2) . . ?
C62 C66 H66A 108.8 . . ?
C62 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?
C26 C27 C35 119.9(3) . . ?
C28 C27 C26 119.0(4) . . ?
C28 C27 C35 121.1(3) . . ?
C6 C1 C2 118.6(3) . . ?
C6 C1 C7 121.4(3) . . ?
C2 C1 C7 120.0(3) . . ?
C41 C42 C44 119.5(3) . . ?
C41 C42 C43 120.4(3) . . ?
C43 C42 C44 120.1(3) . . ?
C41 C40 H40 120.7 . . ?
C39 C40 C41 118.6(3) . . ?
C39 C40 H40 120.7 . . ?
O1 C21 C16 120.2(2) . . ?
O1 C21 C20 122.0(3) . . ?
C16 C21 C20 117.8(3) . . ?
C27 C26 C38 120.4(4) . . ?
C25 C26 C27 119.5(3) . . ?
C25 C26 C38 120.1(3) . . ?
C27 C35 H35 107.0 . . ?
C27 C35 C37 111.9(3) . . ?
C27 C35 C36 114.8(3) . . ?
C37 C35 H35 107.0 . . ?
C36 C35 H35 107.0 . . ?
C36 C35 C37 108.7(3) . . ?
C61 C60 C48 118.3(3) . . ?
C65 C60 C61 120.1(3) . . ?
C65 C60 C48 121.5(3) . . ?
C60 C48 Na2 102.5(2) . . ?
C49 C48 Na2 92.0(2) . . ?
C49 C48 C60 120.0(3) . . ?
C49 C48 C47 119.7(3) . . ?
C47 C48 Na2 72.9(2) . . ?
C47 C48 C60 120.3(3) . . ?
C45 C50 H50 119.0 . . ?
C45 C50 C49 122.0(3) . . ?
C49 C50 H50 119.0 . . ?
C4 C3 Na1 68.66(18) . . ?
C4 C3 C10 120.6(3) . . ?
C2 C3 Na1 86.1(2) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 C10 119.7(3) . . ?
C10 C3 Na1 116.8(3) . . ?
C70 C69 H69 117.2 . . ?
C68 C69 C70 125.6(3) . . ?
C68 C69 H69 117.2 . . ?
C45 C46 H46 118.7 . . ?
C45 C46 C47 122.6(3) . . ?
C47 C46 H46 118.7 . . ?
C1 C2 C3 121.7(3) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C62 C63 H63 119.1 . . ?
C62 C63 C64 121.9(3) . . ?
C64 C63 H63 119.1 . . ?
C50 C45 C51 120.3(3) . . ?
C46 C45 C50 117.7(3) . . ?
C46 C45 C51 122.0(3) . . ?
O2 C43 C42 122.4(3) . . ?
O2 C43 C38 120.2(3) . . ?
C38 C43 C42 117.4(3) . . ?
C48 C49 C57 121.4(3) . . ?
C50 C49 C48 119.2(3) . . ?
C50 C49 C57 119.3(3) . . ?
C45 C51 H51 109.3(16) . . ?
C52 C51 C45 109.9(3) . . ?
C52 C51 H51 110.2(16) . . ?
C53 C51 C45 111.9(3) . . ?
C53 C51 C52 110.7(4) . . ?
C53 C51 H51 104.7(16) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C48 C47 Na2 78.78(19) . . ?
C48 C47 C54 121.4(3) . . ?
C46 C47 Na2 89.2(2) . . ?
C46 C47 C48 118.8(3) . . ?
C46 C47 C54 119.9(3) . . ?
C54 C47 Na2 102.2(2) . . ?
C43 C38 C26 119.2(3) . . ?
C39 C38 C26 120.9(3) . . ?
C39 C38 C43 119.8(3) . . ?
C60 C65 H65 119.1 . . ?
C60 C65 C64 121.8(3) . . ?
C64 C65 H65 119.1 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C40 C39 C38 122.3(3) . . ?
C40 C39 H39 118.9 . . ?
C38 C39 H39 118.9 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C68 C67 H67A 109.5 . . ?
C68 C67 H67B 109.5 . . ?
C68 C67 H67C 109.5 . . ?
C63 C64 H64 121.0 . . ?
C65 C64 C63 118.1(3) . . ?
C65 C64 H64 121.0 . . ?
C1 C7 H7 107.0 . . ?
C8 C7 C1 112.0(3) . . ?
C8 C7 H7 107.0 . . ?
C9 C7 C1 112.2(3) . . ?
C9 C7 H7 107.0 . . ?
C9 C7 C8 111.2(3) . . ?
C47 C54 H54 107.8 . . ?
C56 C54 C47 113.5(3) . . ?
C56 C54 H54 107.8 . . ?
C56 C54 C55 110.3(4) . . ?
C55 C54 C47 109.3(3) . . ?
C55 C54 H54 107.8 . . ?
O4 C68 C69 122.2(3) . . ?
O4 C68 C67 117.7(3) . . ?
C69 C68 C67 120.1(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C27 C28 H28 119.0 . . ?
C27 C28 C23 122.0(4) . . ?
C23 C28 H28 119.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C49 C57 H57 110.5 . . ?
C49 C57 H57A 101.5 . . ?
C49 C57 C58 112.4(5) . . ?
C59 C57 C49 112.7(3) . . ?
C59 C57 H57 110.5 . . ?
C59 C57 H57A 101.5 . . ?
C59 C57 C58 99.7(5) . . ?
C58 C57 H57 110.5 . . ?
C58A C57 C49 106.8(7) . . ?
C58A C57 H57A 101.5 . . ?
C58A C57 C59 128.6(7) . . ?
C26 C25 C32 120.4(3) . . ?
C24 C25 C26 118.8(4) . . ?
C24 C25 C32 120.8(4) . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C3 C10 H10 104.4 . . ?
C3 C10 H10A 104.2 . . ?
C3 C10 C11 110.6(4) . . ?
C3 C10 C12 109.5(4) . . ?
C11 C10 H10 104.4 . . ?
C12 C10 H10A 104.2 . . ?
C12A C10 C3 117.7(6) . . ?
C12A C10 H10 104.4 . . ?
C12A C10 C11 113.7(7) . . ?
C11A C10 C3 117.3(5) . . ?
C11A C10 H10A 104.2 . . ?
C11A C10 C12 115.8(6) . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H30D C30 H30E 109.5 . . ?
H30D C30 H30F 109.5 . . ?
H30E C30 H30F 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C30 H30D 109.5 . . ?
C29 C30 H30E 109.5 . . ?
C29 C30 H30F 109.5 . . ?
C29A C30 H30A 109.5 . . ?
C29A C30 H30B 109.5 . . ?
C29A C30 H30C 109.5 . . ?
C25 C24 H24 118.2 . . ?
C23 C24 C25 123.6(4) . . ?
C23 C24 H24 118.2 . . ?
C25 C32 H32 106.6 . . ?
C34 C32 C25 112.1(4) . . ?
C34 C32 H32 106.6 . . ?
C33 C32 C25 110.1(4) . . ?
C33 C32 H32 106.6 . . ?
C33 C32 C34 114.3(5) . . ?
C28 C23 C29 111.3(5) . . ?
C28 C23 C29A 128.0(6) . . ?
C24 C23 C28 117.1(4) . . ?
C24 C23 C29 130.0(6) . . ?
C24 C23 C29A 113.7(6) . . ?
O6 C75 H75A 109.7 . . ?
O6 C75 H75B 109.7 . . ?
O6 C75 C74 109.9(5) . . ?
H75A C75 H75B 108.2 . . ?
C74 C75 H75A 109.7 . . ?
C74 C75 H75B 109.7 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C29 H29 112.3 . . ?
C23 C29 C30 103.2(7) . . ?
C23 C29 H29 112.3 . . ?
C31 C29 C30 107.5(7) . . ?
C31 C29 C23 108.7(7) . . ?
C31 C29 H29 112.3 . . ?
O6 C72 H72A 110.3 . . ?
O6 C72 H72B 110.3 . . ?
O6 C72 C73 107.1(5) . . ?
H72A C72 H72B 108.6 . . ?
C73 C72 H72A 110.3 . . ?
C73 C72 H72B 110.3 . . ?
C72 C73 H73A 110.9 . . ?
C72 C73 H73B 110.9 . . ?
C72 C73 C74 104.0(5) . . ?
H73A C73 H73B 109.0 . . ?
C74 C73 H73A 110.9 . . ?
C74 C73 H73B 110.9 . . ?
C75 C74 C73 101.2(5) . . ?
C75 C74 H74A 111.5 . . ?
C75 C74 H74B 111.5 . . ?
C73 C74 H74A 111.5 . . ?
C73 C74 H74B 111.5 . . ?
H74A C74 H74B 109.3 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 C29A C23 113.3(8) . . ?
C30 C29A H29A 111.1 . . ?
C30 C29A C31A 106.4(9) . . ?
C23 C29A H29A 111.1 . . ?
C31A C29A C23 103.6(9) . . ?
C31A C29A H29A 111.1 . . ?
C29A C31A H31D 109.5 . . ?
C29A C31A H31E 109.5 . . ?
C29A C31A H31F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C57 C58A H58D 109.5 . . ?
C57 C58A H58E 109.5 . . ?
C57 C58A H58F 109.5 . . ?
H58D C58A H58E 109.5 . . ?
H58D C58A H58F 109.5 . . ?
H58E C58A H58F 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C10 C12A H12D 109.5 . . ?
C10 C12A H12E 109.5 . . ?
C10 C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C10 C11A H11D 109.5 . . ?
C10 C11A H11E 109.5 . . ?
C10 C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.533 0.000 -0.868 1620.6 313.2 ?
2 0.750 0.500 -0.180 1620.6 313.2 ?

_olex2_submission_special_instructions 'No special instructions were received'
