# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_hasj170224b
_database_code_depnum_ccdc_archive 'CCDC 1560715'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_audit_creation_date             2017-02-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H110 Ca2 N4, 2(C6 H6)'
_chemical_formula_sum            'C96 H122 Ca2 N4'
_chemical_formula_weight         1412.13
_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 0.0181 0.0091 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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                   10.3795(3)
_cell_length_b                   10.7062(4)
_cell_length_c                   20.4813(4)
_cell_angle_alpha                101.776(2)
_cell_angle_beta                 91.061(2)
_cell_angle_gamma                115.639(3)
_cell_volume                     1993.93(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3280
_cell_measurement_theta_min      4.4290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             766
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 -6 0.0510
-2 4 -12 0.0358
1 3 9 0.0431
-2 1 -12 0.0288
2 2 -13 0.0354
0 -6 7 0.0682
0 -2 13 0.0378
-5 1 -9 0.0543
0 -1 -12 0.0269
-1 -2 -10 0.0342
5 -5 -6 0.0332
2 -4 -9 0.0309
4 -4 11 0.0401
-1 1 13 0.0263
-4 4 8 0.0363
-6 6 0 0.0417
-4 4 -10 0.0327
3 -2 -11 0.0271
2 5 -6 0.0655
0 1 -13 0.0241
1 -2 13 0.0289
3 -1 12 0.0359
5 -6 5 0.0464

_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18091
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         4.443
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  32.00   1.00   12.50    --  -41.69  77.00 -30.00  105
  2  ω   -114.00 -19.00   1.00   12.50    --  -41.69 -38.00  60.00   95
  3  ω    -64.00  31.00   1.00   12.50    --  -41.69  38.00-120.00   95
  4  ω     23.00  97.00   1.00   12.50    --   41.69-125.00 120.00   74
  5  ω     94.00 178.00   1.00   50.00    --  106.00 125.00  30.00   84
  6  ω     25.00 109.00   1.00   50.00    --  106.00 -94.00 120.00   84
  7  ω     35.00 130.00   1.00   50.00    --  106.00 -45.00 120.00   95
  8  ω     34.00 121.00   1.00   50.00    --  106.00-125.00  30.00   87
  9  ω     82.00 177.00   1.00   50.00    --  106.00  45.00 150.00   95
 10  ω     82.00 177.00   1.00   50.00    --  106.00  45.00-150.00   95
 11  ω     36.00 134.00   1.00   50.00    --  106.00 -61.00   0.00   98
 12  ω     25.00 109.00   1.00   50.00    --  106.00 -94.00-180.00   84
 13  ω     75.00 178.00   1.00   50.00    --  106.00  77.00  90.00  103
 14  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00-180.00   97
 15  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00   0.00   97
 16  ω   -116.00 -20.00   1.00   12.50    --  -41.69 -77.00 120.00   96
 17  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00 -90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6399
_reflns_number_total             7259
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.431
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.033
_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)+(0.0817P)²+0.4017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1314
_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.a Ternary CH refined with riding coordinates:
 C33(H33), C11(H11), C18(H18), C6(H6), C4(H4), C30(H30), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C15(H15), C37(H37), C36(H36), C40(H40), C28(H28),
 C38(H38), C39(H39), C26(H26), C27(H27), C47(H47), C48(H48), C45(H45), C46(H46),
  C43(H43), C44(H44)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_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
Ca1 Ca 0.86108(3) 0.91500(3) 0.88583(2) 0.02005(11) Uani 1 1 d . . . . .
N1 N 0.74386(14) 0.71957(15) 0.79059(7) 0.0187(3) Uani 1 1 d . . . . .
N2 N 0.53465(15) 0.74377(15) 0.77593(7) 0.0210(3) Uani 1 1 d . . . . .
C1 C 0.61136(17) 0.67463(17) 0.75749(8) 0.0178(3) Uani 1 1 d . . . . .
C2 C 0.52660(17) 0.53998(18) 0.69975(8) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.38583(17) 0.44615(19) 0.72605(8) 0.0209(3) Uani 1 1 d . . . . .
H3A H 0.4099 0.4147 0.7637 0.025 Uiso 1 1 calc R . . . .
H3B H 0.3358 0.5027 0.7420 0.025 Uiso 1 1 calc R . . . .
C12 C 0.59594(18) 0.86118(19) 0.83021(8) 0.0211(3) Uani 1 1 d . . . . .
C24 C 0.84674(17) 0.66930(18) 0.77036(8) 0.0207(3) Uani 1 1 d . . . . .
C33 C 0.81331(19) 0.56457(19) 0.87419(9) 0.0247(4) Uani 1 1 d . . . . .
H33 H 0.7989 0.6475 0.8955 0.030 Uiso 1 1 calc R . . . .
C14 C 0.63918(19) 0.9609(2) 0.95076(9) 0.0258(4) Uani 1 1 d . . . . .
H14 H 0.6240 0.9495 0.9942 0.031 Uiso 1 1 calc R . . . .
C8 C 0.60085(17) 0.44502(18) 0.67392(8) 0.0210(3) Uani 1 1 d . . . . .
H8A H 0.6880 0.4999 0.6559 0.025 Uiso 1 1 calc R . . . .
H8B H 0.6277 0.4140 0.7110 0.025 Uiso 1 1 calc R . . . .
C11 C 0.50049(18) 0.31387(19) 0.61902(8) 0.0228(4) Uani 1 1 d . . . . .
H11 H 0.5502 0.2557 0.6033 0.027 Uiso 1 1 calc R . . . .
C29 C 0.88710(18) 0.59849(18) 0.81202(9) 0.0233(4) Uani 1 1 d . . . . .
C16 C 0.7456(2) 1.1140(2) 0.87585(10) 0.0300(4) Uani 1 1 d . . . . .
H16 H 0.8028 1.2045 0.8695 0.036 Uiso 1 1 calc R . . . .
C7 C 0.48192(19) 0.58524(19) 0.63941(8) 0.0238(4) Uani 1 1 d . . . . .
H7A H 0.4323 0.6426 0.6545 0.029 Uiso 1 1 calc R . . . .
H7B H 0.5673 0.6430 0.6211 0.029 Uiso 1 1 calc R . . . .
C15 C 0.7271(2) 1.0951(2) 0.94078(9) 0.0299(4) Uani 1 1 d . . . . .
H15 H 0.7735 1.1720 0.9774 0.036 Uiso 1 1 calc R . . . .
C18 C 0.47647(18) 0.6956(2) 0.90621(9) 0.0258(4) Uani 1 1 d . . . . .
H18 H 0.4956 0.6266 0.8736 0.031 Uiso 1 1 calc R . . . .
C6 C 0.3828(2) 0.4540(2) 0.58432(9) 0.0262(4) Uani 1 1 d . . . . .
H6 H 0.3571 0.4854 0.5465 0.031 Uiso 1 1 calc R . . . .
C25 C 0.92284(18) 0.70625(19) 0.71490(9) 0.0254(4) Uani 1 1 d . . . . .
C17 C 0.6798(2) 0.9994(2) 0.81990(9) 0.0266(4) Uani 1 1 d . . . . .
C9 C 0.36275(19) 0.22428(19) 0.64662(9) 0.0258(4) Uani 1 1 d . . . . .
H9A H 0.3000 0.1421 0.6117 0.031 Uiso 1 1 calc R . . . .
H9B H 0.3865 0.1905 0.6834 0.031 Uiso 1 1 calc R . . . .
C37 C 1.2450(2) 1.0164(2) 0.84721(9) 0.0328(4) Uani 1 1 d . . . . .
H37 H 1.2700 0.9473 0.8242 0.039 Uiso 1 1 calc R . . . .
C41 C 1.12369(18) 1.09304(19) 0.93797(8) 0.0239(4) Uani 1 1 d . . . . .
C13 C 0.57339(18) 0.84297(19) 0.89655(9) 0.0224(4) Uani 1 1 d . . . . .
C4 C 0.28628(18) 0.3159(2) 0.67125(9) 0.0253(4) Uani 1 1 d . . . . .
H4 H 0.1988 0.2595 0.6896 0.030 Uiso 1 1 calc R . . . .
C10 C 0.46049(19) 0.3636(2) 0.56017(9) 0.0263(4) Uani 1 1 d . . . . .
H10A H 0.5469 0.4192 0.5419 0.032 Uiso 1 1 calc R . . . .
H10B H 0.3986 0.2816 0.5249 0.032 Uiso 1 1 calc R . . . .
C36 C 1.15938(19) 0.9881(2) 0.89935(9) 0.0261(4) Uani 1 1 d . . . . .
H36 H 1.1249 0.8988 0.9090 0.031 Uiso 1 1 calc R . . . .
C40 C 1.1660(2) 1.2199(2) 0.91430(9) 0.0289(4) Uani 1 1 d . . . . .
H40 H 1.1365 1.2877 0.9344 0.035 Uiso 1 1 calc R . . . .
C28 C 0.9964(2) 0.5597(2) 0.79477(10) 0.0324(4) Uani 1 1 d . . . . .
H28 H 1.0220 0.5106 0.8209 0.039 Uiso 1 1 calc R . . . .
C5 C 0.24581(19) 0.3653(2) 0.61248(9) 0.0282(4) Uani 1 1 d . . . . .
H5A H 0.1956 0.4221 0.6276 0.034 Uiso 1 1 calc R . . . .
H5B H 0.1822 0.2832 0.5777 0.034 Uiso 1 1 calc R . . . .
C42 C 1.04049(18) 1.07111(18) 0.99321(9) 0.0224(4) Uani 1 1 d . . . . .
C35 C 0.6638(2) 0.4369(2) 0.85685(10) 0.0298(4) Uani 1 1 d . . . . .
H35A H 0.6049 0.4552 0.8271 0.045 Uiso 1 1 calc GR . . . .
H35B H 0.6200 0.4225 0.8973 0.045 Uiso 1 1 calc GR . . . .
H35C H 0.6729 0.3531 0.8353 0.045 Uiso 1 1 calc GR . . . .
C30 C 0.89238(19) 0.7935(2) 0.67243(9) 0.0283(4) Uani 1 1 d . . . . .
H30 H 0.7977 0.7885 0.6805 0.034 Uiso 1 1 calc R . . . .
C38 C 1.2931(2) 1.1455(2) 0.82940(10) 0.0355(5) Uani 1 1 d . . . . .
H38 H 1.3534 1.1657 0.7960 0.043 Uiso 1 1 calc R . . . .
C39 C 1.2489(2) 1.2447(2) 0.86271(10) 0.0349(4) Uani 1 1 d . . . . .
H39 H 1.2764 1.3300 0.8496 0.042 Uiso 1 1 calc R . . . .
C26 C 1.0320(2) 0.6664(2) 0.70083(10) 0.0345(5) Uani 1 1 d . . . . .
H26 H 1.0819 0.6900 0.6645 0.041 Uiso 1 1 calc R . . . .
C19 C 0.3194(2) 0.6639(2) 0.88950(10) 0.0344(4) Uani 1 1 d . . . . .
H19A H 0.2981 0.7316 0.9200 0.052 Uiso 1 1 calc GR . . . .
H19B H 0.2572 0.5693 0.8938 0.052 Uiso 1 1 calc GR . . . .
H19C H 0.3042 0.6708 0.8443 0.052 Uiso 1 1 calc GR . . . .
C22 C 0.6937(3) 1.0208(2) 0.74886(10) 0.0364(5) Uani 1 1 d . . . . .
H22 H 0.7098 0.9431 0.7220 0.044 Uiso 1 1 calc R . . . .
C27 C 1.0676(2) 0.5926(3) 0.73958(11) 0.0408(5) Uani 1 1 d . . . . .
H27 H 1.1395 0.5648 0.7288 0.049 Uiso 1 1 calc R . . . .
C32 C 0.8881(2) 0.7399(3) 0.59635(10) 0.0399(5) Uani 1 1 d . . . . .
H32A H 0.9824 0.7526 0.5863 0.060 Uiso 1 1 calc GR . . . .
H32B H 0.8578 0.7930 0.5726 0.060 Uiso 1 1 calc GR . . . .
H32C H 0.8216 0.6405 0.5827 0.060 Uiso 1 1 calc GR . . . .
C34 C 0.9033(2) 0.5426(2) 0.92678(10) 0.0321(4) Uani 1 1 d . . . . .
H34A H 0.9166 0.4595 0.9085 0.048 Uiso 1 1 calc GR . . . .
H34B H 0.8543 0.5299 0.9660 0.048 Uiso 1 1 calc GR . . . .
H34C H 0.9954 0.6245 0.9388 0.048 Uiso 1 1 calc GR . . . .
C20 C 0.5011(2) 0.6742(2) 0.97578(10) 0.0384(5) Uani 1 1 d . . . . .
H20A H 0.6009 0.6986 0.9861 0.058 Uiso 1 1 calc GR . . . .
H20B H 0.4434 0.5763 0.9766 0.058 Uiso 1 1 calc GR . . . .
H20C H 0.4746 0.7343 1.0085 0.058 Uiso 1 1 calc GR . . . .
C31 C 1.0032(2) 0.9499(2) 0.69460(12) 0.0434(5) Uani 1 1 d . . . . .
H31A H 1.0004 0.9856 0.7413 0.065 Uiso 1 1 calc GR . . . .
H31B H 0.9812 1.0045 0.6684 0.065 Uiso 1 1 calc GR . . . .
H31C H 1.0976 0.9579 0.6881 0.065 Uiso 1 1 calc GR . . . .
C47 C 0.1985(3) -0.3514(3) 0.50649(15) 0.0525(6) Uani 1 1 d . . . . .
H47 H 0.1782 -0.4388 0.5161 0.063 Uiso 1 1 calc R . . . .
C21 C 0.5514(3) 1.0086(3) 0.71876(11) 0.0509(6) Uani 1 1 d . . . . .
H21A H 0.4741 0.9196 0.7219 0.076 Uiso 1 1 calc GR . . . .
H21B H 0.5563 1.0129 0.6724 0.076 Uiso 1 1 calc GR . . . .
H21C H 0.5346 1.0858 0.7431 0.076 Uiso 1 1 calc GR . . . .
C48 C 0.3034(3) -0.2317(3) 0.54522(12) 0.0503(6) Uani 1 1 d . . . . .
H48 H 0.3551 -0.2367 0.5814 0.060 Uiso 1 1 calc R . . . .
C23 C 0.8189(3) 1.1611(3) 0.74399(13) 0.0569(7) Uani 1 1 d . . . . .
H23A H 0.7990 1.2391 0.7642 0.085 Uiso 1 1 calc GR . . . .
H23B H 0.8309 1.1610 0.6976 0.085 Uiso 1 1 calc GR . . . .
H23C H 0.9056 1.1715 0.7671 0.085 Uiso 1 1 calc GR . . . .
C45 C 0.1493(3) -0.2170(4) 0.43976(13) 0.0614(8) Uani 1 1 d . . . . .
H45 H 0.0954 -0.2124 0.4044 0.074 Uiso 1 1 calc R . . . .
C46 C 0.1216(3) -0.3466(3) 0.45357(14) 0.0560(7) Uani 1 1 d . . . . .
H46 H 0.0503 -0.4304 0.4267 0.067 Uiso 1 1 calc R . . . .
C43 C 0.3343(3) -0.1036(3) 0.53185(15) 0.0621(8) Uani 1 1 d . . . . .
H43 H 0.4077 -0.0210 0.5585 0.075 Uiso 1 1 calc R . . . .
C44 C 0.2574(3) -0.0955(3) 0.47884(18) 0.0677(8) Uani 1 1 d . . . . .
H44 H 0.2788 -0.0075 0.4696 0.081 Uiso 1 1 calc R . . . .
H42 H 1.004(2) 1.140(2) 1.0093(10) 0.026(5) 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
Ca1 N1 2.3887(14) . ?
Ca1 C12 2.7289(17) . ?
Ca1 C14 2.8532(17) . ?
Ca1 C16 2.8973(19) . ?
Ca1 C15 2.8998(18) . ?
Ca1 C17 2.8378(18) . ?
Ca1 C41 2.6017(17) . ?
Ca1 C13 2.7677(17) . ?
Ca1 C36 2.8388(18) . ?
Ca1 C42 2.5986(17) . ?
Ca1 C42 2.6131(17) 2_777 ?
N1 C1 1.357(2) . ?
N1 C24 1.423(2) . ?
N2 C1 1.316(2) . ?
N2 C12 1.390(2) . ?
C1 C2 1.555(2) . ?
C2 C3 1.554(2) . ?
C2 C8 1.543(2) . ?
C2 C7 1.548(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.531(2) . ?
C12 C17 1.418(3) . ?
C12 C13 1.421(2) . ?
C24 C29 1.416(3) . ?
C24 C25 1.420(2) . ?
C33 H33 0.9800 . ?
C33 C29 1.524(3) . ?
C33 C35 1.532(3) . ?
C33 C34 1.531(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(3) . ?
C14 C13 1.395(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C11 1.539(2) . ?
C11 H11 0.9800 . ?
C11 C9 1.532(2) . ?
C11 C10 1.531(2) . ?
C29 C28 1.395(2) . ?
C16 H16 0.9300 . ?
C16 C15 1.390(3) . ?
C16 C17 1.399(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.538(2) . ?
C15 H15 0.9300 . ?
C18 H18 0.9800 . ?
C18 C13 1.517(3) . ?
C18 C19 1.531(2) . ?
C18 C20 1.523(3) . ?
C6 H6 0.9800 . ?
C6 C10 1.526(3) . ?
C6 C5 1.530(3) . ?
C25 C30 1.519(3) . ?
C25 C26 1.389(3) . ?
C17 C22 1.519(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C4 1.527(3) . ?
C37 H37 0.9300 . ?
C37 C36 1.399(3) . ?
C37 C38 1.381(3) . ?
C41 C36 1.426(3) . ?
C41 C40 1.426(3) . ?
C41 C42 1.432(2) . ?
C4 H4 0.9800 . ?
C4 C5 1.529(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C36 H36 0.9300 . ?
C40 H40 0.9300 . ?
C40 C39 1.370(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.384(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C42 Ca1 2.6130(17) 2_777 ?
C42 C42 1.475(3) 2_777 ?
C42 H42 0.97(2) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C30 H30 0.9800 . ?
C30 C32 1.540(3) . ?
C30 C31 1.529(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.393(3) . ?
C39 H39 0.9300 . ?
C26 H26 0.9300 . ?
C26 C27 1.374(3) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C22 H22 0.9800 . ?
C22 C21 1.531(3) . ?
C22 C23 1.527(3) . ?
C27 H27 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C47 H47 0.9300 . ?
C47 C48 1.343(4) . ?
C47 C46 1.357(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C48 H48 0.9300 . ?
C48 C43 1.354(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C45 H45 0.9300 . ?
C45 C46 1.380(4) . ?
C45 C44 1.368(4) . ?
C46 H46 0.9300 . ?
C43 H43 0.9300 . ?
C43 C44 1.375(4) . ?
C44 H44 0.9300 . ?

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
N1 Ca1 C12 61.20(5) . . ?
N1 Ca1 C14 106.50(5) . . ?
N1 Ca1 C16 105.51(5) . . ?
N1 Ca1 C15 120.91(5) . . ?
N1 Ca1 C17 77.30(5) . . ?
N1 Ca1 C41 137.46(5) . . ?
N1 Ca1 C13 77.84(5) . . ?
N1 Ca1 C36 108.76(5) . . ?
N1 Ca1 C42 158.25(5) . . ?
N1 Ca1 C42 131.96(5) . 2_777 ?
C12 Ca1 C14 51.56(5) . . ?
C12 Ca1 C16 50.98(5) . . ?
C12 Ca1 C15 59.71(5) . . ?
C12 Ca1 C17 29.43(5) . . ?
C12 Ca1 C13 29.96(5) . . ?
C12 Ca1 C36 160.22(5) . . ?
C14 Ca1 C16 49.43(6) . . ?
C14 Ca1 C15 27.94(6) . . ?
C16 Ca1 C15 27.74(5) . . ?
C17 Ca1 C14 59.08(5) . . ?
C17 Ca1 C16 28.21(5) . . ?
C17 Ca1 C15 50.10(5) . . ?
C17 Ca1 C36 136.19(6) . . ?
C41 Ca1 C12 150.61(6) . . ?
C41 Ca1 C14 115.94(6) . . ?
C41 Ca1 C16 99.93(6) . . ?
C41 Ca1 C15 97.06(6) . . ?
C41 Ca1 C17 122.15(6) . . ?
C41 Ca1 C13 144.63(6) . . ?
C41 Ca1 C36 29.99(6) . . ?
C41 Ca1 C42 58.47(5) . 2_777 ?
C13 Ca1 C14 28.69(5) . . ?
C13 Ca1 C16 59.17(6) . . ?
C13 Ca1 C15 50.56(5) . . ?
C13 Ca1 C17 51.92(5) . . ?
C13 Ca1 C36 169.80(5) . . ?
C36 Ca1 C14 144.11(5) . . ?
C36 Ca1 C16 124.17(6) . . ?
C36 Ca1 C15 126.91(6) . . ?
C42 Ca1 C12 132.46(5) 2_777 . ?
C42 Ca1 C12 138.85(5) . . ?
C42 Ca1 C14 84.32(5) 2_777 . ?
C42 Ca1 C14 89.22(5) . . ?
C42 Ca1 C16 115.76(6) 2_777 . ?
C42 Ca1 C16 96.11(6) . . ?
C42 Ca1 C15 79.84(5) . . ?
C42 Ca1 C15 90.57(6) 2_777 . ?
C42 Ca1 C17 124.27(6) . . ?
C42 Ca1 C17 140.42(6) 2_777 . ?
C42 Ca1 C41 31.96(5) . . ?
C42 Ca1 C13 102.55(5) 2_777 . ?
C42 Ca1 C13 116.42(5) . . ?
C42 Ca1 C36 67.24(5) 2_777 . ?
C42 Ca1 C36 55.00(5) . . ?
C42 Ca1 C42 32.89(7) . 2_777 ?
C1 N1 Ca1 127.15(11) . . ?
C1 N1 C24 126.14(14) . . ?
C24 N1 Ca1 106.35(10) . . ?
C1 N2 C12 116.64(14) . . ?
N1 C1 C2 128.27(14) . . ?
N2 C1 N1 120.14(15) . . ?
N2 C1 C2 111.49(14) . . ?
C3 C2 C1 106.73(12) . . ?
C8 C2 C1 117.66(13) . . ?
C8 C2 C3 107.38(14) . . ?
C8 C2 C7 108.38(13) . . ?
C7 C2 C1 109.14(13) . . ?
C7 C2 C3 107.06(13) . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 111.67(13) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N2 C12 Ca1 114.83(10) . . ?
N2 C12 C17 120.52(15) . . ?
N2 C12 C13 119.81(16) . . ?
C17 C12 Ca1 79.54(10) . . ?
C17 C12 C13 119.66(16) . . ?
C13 C12 Ca1 76.53(9) . . ?
C29 C24 N1 118.64(15) . . ?
C29 C24 C25 119.81(15) . . ?
C25 C24 N1 120.96(16) . . ?
C29 C33 H33 106.7 . . ?
C29 C33 C35 112.55(15) . . ?
C29 C33 C34 113.87(15) . . ?
C35 C33 H33 106.7 . . ?
C34 C33 H33 106.7 . . ?
C34 C33 C35 109.81(15) . . ?
Ca1 C14 H14 121.5 . . ?
C15 C14 Ca1 77.90(10) . . ?
C15 C14 H14 119.5 . . ?
C15 C14 C13 120.98(17) . . ?
C13 C14 Ca1 72.25(9) . . ?
C13 C14 H14 119.5 . . ?
C2 C8 H8A 109.4 . . ?
C2 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C11 C8 C2 110.99(13) . . ?
C11 C8 H8A 109.4 . . ?
C11 C8 H8B 109.4 . . ?
C8 C11 H11 109.4 . . ?
C9 C11 C8 110.42(14) . . ?
C9 C11 H11 109.4 . . ?
C10 C11 C8 109.15(14) . . ?
C10 C11 H11 109.4 . . ?
C10 C11 C9 109.07(14) . . ?
C24 C29 C33 121.21(15) . . ?
C28 C29 C24 118.35(17) . . ?
C28 C29 C33 120.44(17) . . ?
Ca1 C16 H16 122.1 . . ?
C15 C16 Ca1 76.23(11) . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.23(18) . . ?
C17 C16 Ca1 73.53(10) . . ?
C17 C16 H16 119.4 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 108.0 . . ?
C6 C7 C2 110.90(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
Ca1 C15 H15 120.9 . . ?
C14 C15 Ca1 74.17(10) . . ?
C14 C15 C16 119.80(17) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 Ca1 76.03(11) . . ?
C16 C15 H15 120.1 . . ?
C13 C18 H18 107.6 . . ?
C13 C18 C19 108.83(15) . . ?
C13 C18 C20 114.38(16) . . ?
C19 C18 H18 107.6 . . ?
C20 C18 H18 107.6 . . ?
C20 C18 C19 110.69(15) . . ?
C7 C6 H6 109.4 . . ?
C10 C6 C7 109.67(15) . . ?
C10 C6 H6 109.4 . . ?
C10 C6 C5 109.50(15) . . ?
C5 C6 C7 109.55(14) . . ?
C5 C6 H6 109.4 . . ?
C24 C25 C30 121.77(15) . . ?
C26 C25 C24 119.03(18) . . ?
C26 C25 C30 119.14(17) . . ?
C12 C17 Ca1 71.02(9) . . ?
C12 C17 C22 119.70(16) . . ?
C16 C17 Ca1 78.26(11) . . ?
C16 C17 C12 118.91(17) . . ?
C16 C17 C22 121.37(18) . . ?
C22 C17 Ca1 122.52(13) . . ?
C11 C9 H9A 109.9 . . ?
C11 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C4 C9 C11 109.04(15) . . ?
C4 C9 H9A 109.9 . . ?
C4 C9 H9B 109.9 . . ?
C36 C37 H37 119.5 . . ?
C38 C37 H37 119.5 . . ?
C38 C37 C36 121.01(19) . . ?
C36 C41 Ca1 84.24(10) . . ?
C36 C41 C42 123.67(17) . . ?
C40 C41 Ca1 109.07(12) . . ?
C40 C41 C36 115.21(16) . . ?
C40 C41 C42 120.90(17) . . ?
C42 C41 Ca1 73.90(10) . . ?
C12 C13 Ca1 73.51(9) . . ?
C12 C13 C18 118.80(16) . . ?
C14 C13 Ca1 79.06(10) . . ?
C14 C13 C12 119.28(17) . . ?
C14 C13 C18 121.92(16) . . ?
C18 C13 Ca1 118.54(11) . . ?
C3 C4 H4 109.4 . . ?
C9 C4 C3 109.82(14) . . ?
C9 C4 H4 109.4 . . ?
C9 C4 C5 109.44(14) . . ?
C5 C4 C3 109.40(15) . . ?
C5 C4 H4 109.4 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C6 C10 C11 109.62(14) . . ?
C6 C10 H10A 109.7 . . ?
C6 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
Ca1 C36 H36 81.6 . . ?
C37 C36 Ca1 123.59(13) . . ?
C37 C36 C41 121.45(18) . . ?
C37 C36 H36 119.3 . . ?
C41 C36 Ca1 65.76(9) . . ?
C41 C36 H36 119.3 . . ?
C41 C40 H40 119.1 . . ?
C39 C40 C41 121.83(19) . . ?
C39 C40 H40 119.1 . . ?
C29 C28 H28 119.2 . . ?
C27 C28 C29 121.54(19) . . ?
C27 C28 H28 119.2 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
C4 C5 C6 109.22(14) . . ?
C4 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
Ca1 C42 Ca1 147.11(7) . 2_777 ?
Ca1 C42 H42 93.0(12) 2_777 . ?
Ca1 C42 H42 101.2(12) . . ?
C41 C42 Ca1 74.14(10) . . ?
C41 C42 Ca1 125.03(12) . 2_777 ?
C41 C42 C42 122.4(2) . 2_777 ?
C41 C42 H42 116.7(13) . . ?
C42 C42 Ca1 73.02(13) 2_777 2_777 ?
C42 C42 Ca1 74.10(13) 2_777 . ?
C42 C42 H42 115.9(13) 2_777 . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C25 C30 H30 107.6 . . ?
C25 C30 C32 114.16(17) . . ?
C25 C30 C31 110.21(16) . . ?
C32 C30 H30 107.6 . . ?
C31 C30 H30 107.6 . . ?
C31 C30 C32 109.44(17) . . ?
C37 C38 H38 120.9 . . ?
C37 C38 C39 118.29(17) . . ?
C39 C38 H38 120.9 . . ?
C40 C39 C38 121.73(19) . . ?
C40 C39 H39 119.1 . . ?
C38 C39 H39 119.1 . . ?
C25 C26 H26 119.4 . . ?
C27 C26 C25 121.28(19) . . ?
C27 C26 H26 119.4 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C22 H22 107.7 . . ?
C17 C22 C21 109.11(18) . . ?
C17 C22 C23 113.93(18) . . ?
C21 C22 H22 107.7 . . ?
C23 C22 H22 107.7 . . ?
C23 C22 C21 110.6(2) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 C28 119.88(17) . . ?
C26 C27 H27 120.1 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C48 C47 H47 119.5 . . ?
C48 C47 C46 120.9(3) . . ?
C46 C47 H47 119.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C47 C48 H48 119.9 . . ?
C47 C48 C43 120.2(2) . . ?
C43 C48 H48 119.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C46 C45 H45 120.5 . . ?
C44 C45 H45 120.5 . . ?
C44 C45 C46 119.0(2) . . ?
C47 C46 C45 119.8(2) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C48 C43 H43 120.0 . . ?
C48 C43 C44 120.1(3) . . ?
C44 C43 H43 120.0 . . ?
C45 C44 C43 119.8(3) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2017-02-24
_olex2_submission_original_sample_id hasj170224b
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
####################################################################### 
# 
# 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_hasj150420c
_database_code_depnum_ccdc_archive 'CCDC 1560714'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_audit_creation_date             2017-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H98 Ca2 N4, 4(C6 H6)'
_chemical_formula_sum            'C96 H122 Ca2 N4'
_chemical_formula_weight         1412.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ca H N C '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.43516(13)
_cell_length_b                   10.43114(11)
_cell_length_c                   27.6902(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.7627(10)
_cell_angle_gamma                90
_cell_volume                     4096.11(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7946
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.4470
_cell_measurement_theta_min      4.0450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -7 1 0.2159
6 -5 3 0.1437
5 -6 2 0.1516
-7 4 -3 0.1607
5 -3 11 0.1517
8 -4 -1 0.1444
-4 6 -2 0.1494
9 0 3 0.1424
-8 3 7 0.1421
0 1 -17 0.0856
2 0 -18 0.0871
-3 1 18 0.0666
9 0 1 0.1362
5 6 -1 0.1587
0 7 -3 0.1277
-2 -7 2 0.2248
-9 0 -2 0.1209
0 0 -18 0.0715

_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 -7.0000 1.0002 0.1892 0.8322 0.5867
6.0000 -5.0000 2.9999 0.0758 0.2193 0.9921
5.0000 -6.0000 2.0000 0.0744 0.4157 0.9673
-7.0000 4.0000 -2.9999 -0.0269 -0.0426 -0.9997
5.0000 -3.0000 11.0000 0.4674 -0.1265 0.8775
8.0000 -4.0000 -1.0002 -0.2032 0.0662 1.0202
-4.0000 6.0000 -2.0001 -0.1034 -0.4707 -0.8784
9.0000 0.0000 2.9997 -0.1105 -0.5543 0.8522
-8.0000 3.0000 7.0003 0.5248 -0.0626 -0.8360
-0.0000 1.0000 -17.0002 -0.8746 0.2128 -0.3726
2.0000 -0.0000 -18.0002 -0.9631 0.2441 -0.1304
-3.0000 1.0000 18.0002 0.9723 -0.3107 -0.0399
9.0000 0.0000 0.9997 -0.2111 -0.5149 0.8180
5.0000 6.0000 -1.0004 -0.3145 -0.9856 -0.0604
-0.0000 7.0000 -3.0003 -0.2897 -0.7928 -0.6209
-2.0000 -7.0000 2.0003 0.2975 0.9226 0.4258
-9.0000 -0.0000 -1.9997 0.1608 0.5346 -0.8351
-0.0000 -0.0000 -18.0001 -0.9050 0.3541 -0.3084

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14535
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.565
_diffrn_reflns_theta_min         3.234
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  30.00   1.00    1.00    --  -41.69  38.00 -60.00   80
  2  ω    -79.00  37.00   1.00    1.00    --  -41.69  19.00-150.00  116
  3  ω     31.00  65.00   1.00    2.00    --  106.00 -30.00-120.00   34
  4  ω     25.00 109.00   1.00    2.00    --  106.00 -94.00-120.00   84
  5  ω     75.00 178.00   1.00    2.00    --  106.00  77.00 -60.00  103
  6  ω     98.00 174.00   1.00    2.00    --  106.00 125.00-120.00   76
  7  ω     79.00 170.00   1.00    2.00    --  106.00  77.00-120.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0290402000
_diffrn_orient_matrix_UB_12      -0.0198414000
_diffrn_orient_matrix_UB_13      0.0502793000
_diffrn_orient_matrix_UB_21      -0.0550271000
_diffrn_orient_matrix_UB_22      -0.1216940000
_diffrn_orient_matrix_UB_23      -0.0196740000
_diffrn_orient_matrix_UB_31      0.0889819000
_diffrn_orient_matrix_UB_32      -0.0813612000
_diffrn_orient_matrix_UB_33      0.0171334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7231
_reflns_number_total             7922
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7922
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.029
_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)+(0.0530P)²+1.0947P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1040
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C20(H20), C21(H21), C22(H22), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Ca1 Ca 0.87718(2) 0.09474(2) 0.04210(2) 0.01863(8) Uani 1 1 d . . . . .
N1 N 0.79843(7) 0.33506(10) 0.11631(4) 0.0179(2) Uani 1 1 d . . . . .
N2 N 0.82492(7) 0.11513(10) 0.11849(4) 0.0166(2) Uani 1 1 d . . . . .
C1 C 0.82702(9) 0.33316(12) 0.07097(5) 0.0191(3) Uani 1 1 d . . . . .
C2 C 0.75902(10) 0.32128(13) 0.02690(5) 0.0227(3) Uani 1 1 d . . . . .
C3 C 0.79012(11) 0.30893(14) -0.01775(5) 0.0288(3) Uani 1 1 d . . . . .
H3 H 0.745320 0.297102 -0.047222 0.035 Uiso 1 1 calc R . . . .
C4 C 0.88599(12) 0.31372(15) -0.01969(6) 0.0309(3) Uani 1 1 d . . . . .
H4 H 0.906144 0.301753 -0.050130 0.037 Uiso 1 1 calc R . . . .
C5 C 0.95184(11) 0.33594(13) 0.02280(6) 0.0266(3) Uani 1 1 d . . . . .
H5 H 1.016530 0.344933 0.020845 0.032 Uiso 1 1 calc R . . . .
C6 C 0.92420(9) 0.34530(12) 0.06855(5) 0.0211(3) Uani 1 1 d . . . . .
C7 C 0.99465(9) 0.37419(13) 0.11511(5) 0.0226(3) Uani 1 1 d . . . . .
H7 H 0.971242 0.332752 0.143115 0.027 Uiso 1 1 calc R . . . .
C8 C 0.99419(14) 0.51794(16) 0.12308(7) 0.0425(4) Uani 1 1 d . . . . .
H8A H 1.014287 0.561356 0.095383 0.064 Uiso 1 1 calc GR . . . .
H8B H 1.037632 0.539534 0.153599 0.064 Uiso 1 1 calc GR . . . .
H8C H 0.930345 0.545872 0.125395 0.064 Uiso 1 1 calc GR . . . .
H30 H 0.9603(14) 0.070(2) -0.0473(7) 0.041(5) Uiso 1 1 d . . . . .
C9 C 1.09347(11) 0.3242(2) 0.11523(8) 0.0485(5) Uani 1 1 d . . . . .
H9A H 1.090976 0.231607 0.109223 0.073 Uiso 1 1 calc GR . . . .
H9B H 1.133498 0.341705 0.147211 0.073 Uiso 1 1 calc GR . . . .
H9C H 1.119718 0.367172 0.089316 0.073 Uiso 1 1 calc GR . . . .
C10 C 0.65480(10) 0.32832(14) 0.02906(5) 0.0250(3) Uani 1 1 d . . . . .
H10 H 0.642800 0.269272 0.055674 0.030 Uiso 1 1 calc R . . . .
C11 C 0.63064(10) 0.46575(14) 0.04310(6) 0.0310(3) Uani 1 1 d . . . . .
H11A H 0.671183 0.489751 0.074242 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.564447 0.469477 0.046714 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.640953 0.525339 0.017255 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.58946(11) 0.28891(16) -0.01877(6) 0.0348(4) Uani 1 1 d . . . . .
H12A H 0.595356 0.350667 -0.044695 0.052 Uiso 1 1 calc GR . . . .
H12B H 0.524094 0.287475 -0.013664 0.052 Uiso 1 1 calc GR . . . .
H12C H 0.607136 0.203371 -0.028552 0.052 Uiso 1 1 calc GR . . . .
C13 C 0.79649(8) 0.22393(12) 0.13831(4) 0.0159(2) Uani 1 1 d . . . . .
C14 C 0.76516(9) 0.23834(13) 0.18904(5) 0.0197(3) Uani 1 1 d . . . . .
C15 C 0.67074(10) 0.31069(15) 0.18107(6) 0.0288(3) Uani 1 1 d . . . . .
H15A H 0.677388 0.392535 0.164672 0.043 Uiso 1 1 calc GR . . . .
H15B H 0.652616 0.326778 0.212912 0.043 Uiso 1 1 calc GR . . . .
H15C H 0.622036 0.258881 0.160532 0.043 Uiso 1 1 calc GR . . . .
C16 C 0.83933(10) 0.32272(14) 0.22146(5) 0.0260(3) Uani 1 1 d . . . . .
H16A H 0.900840 0.280017 0.226263 0.039 Uiso 1 1 calc GR . . . .
H16B H 0.821000 0.336247 0.253413 0.039 Uiso 1 1 calc GR . . . .
H16C H 0.843381 0.405629 0.205336 0.039 Uiso 1 1 calc GR . . . .
C17 C 0.75343(11) 0.11476(14) 0.21725(5) 0.0266(3) Uani 1 1 d . . . . .
H17A H 0.702198 0.063422 0.198476 0.040 Uiso 1 1 calc GR . . . .
H17B H 0.738348 0.136349 0.249352 0.040 Uiso 1 1 calc GR . . . .
H17C H 0.812243 0.065505 0.221966 0.040 Uiso 1 1 calc GR . . . .
C18 C 0.81108(9) -0.01279(12) 0.13330(4) 0.0168(2) Uani 1 1 d . . . . .
C19 C 0.89033(10) -0.08912(12) 0.15289(5) 0.0207(3) Uani 1 1 d . . . . .
C20 C 0.87641(11) -0.21830(13) 0.16275(5) 0.0260(3) Uani 1 1 d . . . . .
H20 H 0.929087 -0.269093 0.177002 0.031 Uiso 1 1 calc R . . . .
C21 C 0.78813(11) -0.27432(13) 0.15235(5) 0.0273(3) Uani 1 1 d . . . . .
H21 H 0.780419 -0.362625 0.159009 0.033 Uiso 1 1 calc R . . . .
C22 C 0.71099(10) -0.19999(13) 0.13208(5) 0.0247(3) Uani 1 1 d . . . . .
H22 H 0.650324 -0.238405 0.124643 0.030 Uiso 1 1 calc R . . . .
C23 C 0.72064(9) -0.07056(13) 0.12244(5) 0.0195(3) Uani 1 1 d . . . . .
C24 C 0.63555(9) 0.00664(13) 0.09821(5) 0.0233(3) Uani 1 1 d . . . . .
H24 H 0.649376 0.099097 0.105965 0.028 Uiso 1 1 calc R . . . .
C25 C 0.54447(11) -0.02766(17) 0.11615(7) 0.0373(4) Uani 1 1 d . . . . .
H25A H 0.525238 -0.114937 0.105634 0.056 Uiso 1 1 calc GR . . . .
H25B H 0.494612 0.032718 0.102177 0.056 Uiso 1 1 calc GR . . . .
H25C H 0.555308 -0.022718 0.152106 0.056 Uiso 1 1 calc GR . . . .
C26 C 0.62059(10) -0.00892(15) 0.04240(6) 0.0293(3) Uani 1 1 d . . . . .
H26A H 0.677525 0.018466 0.030740 0.044 Uiso 1 1 calc GR . . . .
H26B H 0.567064 0.043883 0.026928 0.044 Uiso 1 1 calc GR . . . .
H26C H 0.607600 -0.099091 0.033758 0.044 Uiso 1 1 calc GR . . . .
C27 C 0.98908(10) -0.03293(14) 0.16424(6) 0.0270(3) Uani 1 1 d . . . . .
H27 H 0.991413 0.039882 0.141005 0.032 Uiso 1 1 calc R . . . .
C28 C 1.01021(12) 0.0211(2) 0.21634(8) 0.0534(6) Uani 1 1 d . . . . .
H28A H 0.964976 0.089212 0.219499 0.080 Uiso 1 1 calc GR . . . .
H28B H 1.074312 0.056156 0.223096 0.080 Uiso 1 1 calc GR . . . .
H28C H 1.004918 -0.047423 0.239892 0.080 Uiso 1 1 calc GR . . . .
C29 C 1.06659(11) -0.12786(16) 0.15777(6) 0.0307(3) Uani 1 1 d . . . . .
H29A H 1.072672 -0.193272 0.183572 0.046 Uiso 1 1 calc GR . . . .
H29B H 1.126548 -0.082090 0.160100 0.046 Uiso 1 1 calc GR . . . .
H29C H 1.050200 -0.169030 0.125489 0.046 Uiso 1 1 calc GR . . . .
C30 C 0.96558(10) -0.00872(15) -0.02251(5) 0.0254(3) Uani 1 1 d . . . . .
C31 C 0.87987(9) -0.08066(13) -0.02515(5) 0.0227(3) Uani 1 1 d . . . . .
C32 C 0.80212(10) -0.06196(15) -0.06462(6) 0.0281(3) Uani 1 1 d . . . . .
H32 H 0.806407 0.001573 -0.088687 0.034 Uiso 1 1 calc R . . . .
C33 C 0.72076(11) -0.13400(18) -0.06870(6) 0.0354(4) Uani 1 1 d . . . . .
H33 H 0.671078 -0.120828 -0.096011 0.042 Uiso 1 1 calc R . . . .
C34 C 0.71017(11) -0.22568(17) -0.03352(7) 0.0377(4) Uani 1 1 d . . . . .
H34 H 0.654928 -0.277028 -0.037320 0.045 Uiso 1 1 calc R . . . .
C35 C 0.78096(11) -0.24045(15) 0.00672(6) 0.0326(3) Uani 1 1 d . . . . .
H35 H 0.773626 -0.300867 0.031405 0.039 Uiso 1 1 calc R . . . .
C36 C 0.86378(10) -0.16786(14) 0.01194(5) 0.0261(3) Uani 1 1 d . . . . .
H36 H 0.910315 -0.177020 0.040907 0.031 Uiso 1 1 calc R . . . .
C43 C 0.43228(13) 0.48323(17) 0.13344(6) 0.0380(4) Uani 1 1 d . . . . .
H43 H 0.462240 0.409830 0.123045 0.046 Uiso 1 1 calc R . . . .
C44 C 0.33506(12) 0.48813(17) 0.12700(6) 0.0368(4) Uani 1 1 d . . . . .
H44 H 0.298157 0.418550 0.111879 0.044 Uiso 1 1 calc R . . . .
C45 C 0.29173(12) 0.59421(18) 0.14256(6) 0.0370(4) Uani 1 1 d . . . . .
H45 H 0.224977 0.596826 0.138747 0.044 Uiso 1 1 calc R . . . .
C46 C 0.34503(13) 0.69669(17) 0.16368(6) 0.0400(4) Uani 1 1 d . . . . .
H46 H 0.315002 0.770316 0.173847 0.048 Uiso 1 1 calc R . . . .
C47 C 0.44237(13) 0.69164(17) 0.16996(6) 0.0410(4) Uani 1 1 d . . . . .
H47 H 0.479309 0.761729 0.184609 0.049 Uiso 1 1 calc R . . . .
C48 C 0.48581(12) 0.58470(17) 0.15492(6) 0.0389(4) Uani 1 1 d . . . . .
H48 H 0.552634 0.581099 0.159398 0.047 Uiso 1 1 calc R . . . .
C37 C 0.43565(12) 0.1727(2) 0.21533(6) 0.0419(4) Uani 1 1 d . . . . .
H37 H 0.481429 0.227967 0.205855 0.050 Uiso 1 1 calc R . . . .
C38 C 0.46209(13) 0.0550(2) 0.23491(7) 0.0469(5) Uani 1 1 d . . . . .
H38 H 0.526143 0.028909 0.239140 0.056 Uiso 1 1 calc R . . . .
C39 C 0.39575(15) -0.02586(18) 0.24854(7) 0.0460(4) Uani 1 1 d . . . . .
H39 H 0.413979 -0.107870 0.261947 0.055 Uiso 1 1 calc R . . . .
C40 C 0.30312(14) 0.01270(19) 0.24263(8) 0.0488(5) Uani 1 1 d . . . . .
H40 H 0.257151 -0.042529 0.251937 0.059 Uiso 1 1 calc R . . . .
C41 C 0.27744(12) 0.1319(2) 0.22314(8) 0.0490(5) Uani 1 1 d . . . . .
H41 H 0.213643 0.158956 0.219290 0.059 Uiso 1 1 calc R . . . .
C42 C 0.34320(13) 0.21153(17) 0.20929(7) 0.0400(4) Uani 1 1 d . . . . .
H42 H 0.325026 0.293236 0.195567 0.048 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
Ca1 N2 2.3841(11) . ?
Ca1 C1 2.7503(13) . ?
Ca1 C2 2.8987(14) . ?
Ca1 C3 2.9223(15) . ?
Ca1 C4 2.8710(15) . ?
Ca1 C5 2.8272(14) . ?
Ca1 C6 2.7645(13) . ?
Ca1 C30 2.5907(14) 3_755 ?
Ca1 C30 2.6166(14) . ?
Ca1 C31 2.6160(13) . ?
Ca1 C36 2.8598(15) . ?
N1 C1 1.3930(17) . ?
N1 C13 1.3122(17) . ?
N2 C13 1.3571(16) . ?
N2 C18 1.4211(16) . ?
C1 C2 1.4215(19) . ?
C1 C6 1.4224(18) . ?
C2 C3 1.398(2) . ?
C2 C10 1.5186(19) . ?
C3 H3 0.9500 . ?
C3 C4 1.396(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.401(2) . ?
C6 C7 1.5157(19) . ?
C7 H7 1.0000 . ?
C7 C8 1.516(2) . ?
C7 C9 1.518(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.542(2) . ?
C10 C12 1.532(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.5614(17) . ?
C14 C15 1.5374(18) . ?
C14 C16 1.5387(18) . ?
C14 C17 1.5330(19) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.4160(18) . ?
C18 C23 1.4182(18) . ?
C19 C20 1.3969(19) . ?
C19 C27 1.5189(19) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.3882(19) . ?
C23 C24 1.5165(19) . ?
C24 H24 1.0000 . ?
C24 C25 1.532(2) . ?
C24 C26 1.528(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.526(2) . ?
C27 C29 1.529(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 1.07(2) . ?
C30 C30 1.453(3) 3_755 ?
C30 C31 1.4372(19) . ?
C31 C32 1.426(2) . ?
C31 C36 1.423(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.394(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.373(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.400(2) . ?
C36 H36 0.9500 . ?
C43 H43 0.9500 . ?
C43 C44 1.382(2) . ?
C43 C48 1.378(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.379(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.381(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.384(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.381(3) . ?
C48 H48 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.367(3) . ?
C37 C42 1.375(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.381(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.377(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.378(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.369(3) . ?
C42 H42 0.9500 . ?

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
N2 Ca1 C1 61.15(4) . . ?
N2 Ca1 C2 77.35(4) . . ?
N2 Ca1 C3 105.13(4) . . ?
N2 Ca1 C4 120.95(4) . . ?
N2 Ca1 C5 106.46(4) . . ?
N2 Ca1 C6 77.49(4) . . ?
N2 Ca1 C30 130.66(4) . 3_755 ?
N2 Ca1 C30 156.77(4) . . ?
N2 Ca1 C31 138.00(4) . . ?
N2 Ca1 C36 109.22(4) . . ?
C1 Ca1 C2 29.00(4) . . ?
C1 Ca1 C3 50.56(4) . . ?
C1 Ca1 C4 59.81(4) . . ?
C1 Ca1 C5 51.72(4) . . ?
C1 Ca1 C6 29.89(4) . . ?
C1 Ca1 C36 160.72(4) . . ?
C2 Ca1 C3 27.78(4) . . ?
C4 Ca1 C2 49.85(4) . . ?
C4 Ca1 C3 27.86(4) . . ?
C5 Ca1 C2 58.79(4) . . ?
C5 Ca1 C3 49.54(4) . . ?
C5 Ca1 C4 28.16(5) . . ?
C5 Ca1 C36 143.57(4) . . ?
C6 Ca1 C2 51.42(4) . . ?
C6 Ca1 C3 59.05(4) . . ?
C6 Ca1 C4 50.93(4) . . ?
C6 Ca1 C5 28.99(4) . . ?
C6 Ca1 C36 169.37(4) . . ?
C30 Ca1 C1 131.49(4) 3_755 . ?
C30 Ca1 C1 139.47(4) . . ?
C30 Ca1 C2 140.06(4) 3_755 . ?
C30 Ca1 C2 125.86(4) . . ?
C30 Ca1 C3 116.54(5) 3_755 . ?
C30 Ca1 C3 98.08(5) . . ?
C30 Ca1 C4 80.74(5) . . ?
C30 Ca1 C4 90.73(5) 3_755 . ?
C30 Ca1 C5 83.61(5) 3_755 . ?
C30 Ca1 C5 89.20(4) . . ?
C30 Ca1 C6 101.63(4) 3_755 . ?
C30 Ca1 C6 116.37(4) . . ?
C30 Ca1 C30 32.40(6) 3_755 . ?
C30 Ca1 C31 58.58(4) 3_755 . ?
C30 Ca1 C36 67.74(4) 3_755 . ?
C30 Ca1 C36 54.57(4) . . ?
C31 Ca1 C1 151.52(4) . . ?
C31 Ca1 C2 123.59(4) . . ?
C31 Ca1 C3 101.13(4) . . ?
C31 Ca1 C4 97.13(5) . . ?
C31 Ca1 C5 115.53(4) . . ?
C31 Ca1 C6 144.52(4) . . ?
C31 Ca1 C30 31.88(4) . . ?
C31 Ca1 C36 29.70(4) . . ?
C36 Ca1 C2 137.10(4) . . ?
C36 Ca1 C3 124.63(4) . . ?
C36 Ca1 C4 126.60(4) . . ?
C13 N1 C1 116.20(11) . . ?
C13 N2 Ca1 127.09(8) . . ?
C13 N2 C18 126.80(11) . . ?
C18 N2 Ca1 104.91(7) . . ?
N1 C1 Ca1 114.40(8) . . ?
N1 C1 C2 120.11(12) . . ?
N1 C1 C6 120.12(12) . . ?
C2 C1 Ca1 81.30(8) . . ?
C2 C1 C6 119.76(12) . . ?
C6 C1 Ca1 75.61(7) . . ?
C1 C2 Ca1 69.70(7) . . ?
C1 C2 C10 119.49(12) . . ?
C3 C2 Ca1 77.05(8) . . ?
C3 C2 C1 118.88(13) . . ?
C3 C2 C10 121.57(13) . . ?
C10 C2 Ca1 126.45(9) . . ?
Ca1 C3 H3 122.7 . . ?
C2 C3 Ca1 75.17(8) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 Ca1 74.02(9) . . ?
C4 C3 C2 121.01(14) . . ?
C4 C3 H3 119.5 . . ?
Ca1 C4 H4 118.6 . . ?
C3 C4 Ca1 78.11(9) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 Ca1 74.16(8) . . ?
C5 C4 C3 120.05(14) . . ?
C5 C4 H4 120.0 . . ?
Ca1 C5 H5 120.8 . . ?
C4 C5 Ca1 77.68(9) . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.85(13) . . ?
C6 C5 Ca1 73.02(8) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 Ca1 74.50(7) . . ?
C1 C6 C7 119.25(12) . . ?
C5 C6 Ca1 77.99(8) . . ?
C5 C6 C1 119.09(13) . . ?
C5 C6 C7 121.60(12) . . ?
C7 C6 Ca1 120.39(9) . . ?
C6 C7 H7 107.7 . . ?
C6 C7 C8 107.45(12) . . ?
C6 C7 C9 114.48(12) . . ?
C8 C7 H7 107.7 . . ?
C8 C7 C9 111.64(14) . . ?
C9 C7 H7 107.7 . . ?
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 . . ?
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 . . ?
C2 C10 H10 108.0 . . ?
C2 C10 C11 109.10(11) . . ?
C2 C10 C12 114.04(13) . . ?
C11 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C12 C10 C11 109.62(12) . . ?
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 . . ?
N1 C13 N2 121.11(11) . . ?
N1 C13 C14 111.57(11) . . ?
N2 C13 C14 127.20(11) . . ?
C15 C14 C13 108.42(11) . . ?
C15 C14 C16 107.73(11) . . ?
C16 C14 C13 107.04(10) . . ?
C17 C14 C13 117.11(11) . . ?
C17 C14 C15 107.86(11) . . ?
C17 C14 C16 108.35(11) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 119.43(11) . . ?
C19 C18 C23 119.22(12) . . ?
C23 C18 N2 120.75(11) . . ?
C18 C19 C27 121.48(12) . . ?
C20 C19 C18 118.81(13) . . ?
C20 C19 C27 119.70(12) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 C19 121.85(13) . . ?
C21 C20 H20 119.1 . . ?
C20 C21 H21 120.4 . . ?
C20 C21 C22 119.16(13) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 119.3 . . ?
C21 C22 C23 121.32(13) . . ?
C23 C22 H22 119.3 . . ?
C18 C23 C24 120.37(12) . . ?
C22 C23 C18 119.60(12) . . ?
C22 C23 C24 119.97(12) . . ?
C23 C24 H24 107.7 . . ?
C23 C24 C25 113.93(13) . . ?
C23 C24 C26 109.93(11) . . ?
C25 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C26 C24 C25 109.58(12) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 H27 107.6 . . ?
C19 C27 C28 110.63(13) . . ?
C19 C27 C29 113.88(12) . . ?
C28 C27 H27 107.6 . . ?
C28 C27 C29 109.17(12) . . ?
C29 C27 H27 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Ca1 C30 Ca1 147.60(6) 3_755 . ?
Ca1 C30 H30 97.8(11) . . ?
Ca1 C30 H30 95.4(11) 3_755 . ?
C30 C30 Ca1 74.78(11) 3_755 3_755 ?
C30 C30 Ca1 72.82(10) 3_755 . ?
C30 C30 H30 114.2(11) 3_755 . ?
C31 C30 Ca1 74.03(8) . . ?
C31 C30 Ca1 126.03(10) . 3_755 ?
C31 C30 H30 114.4(11) . . ?
C31 C30 C30 123.60(16) . 3_755 ?
C30 C31 Ca1 74.08(8) . . ?
C32 C31 Ca1 109.62(9) . . ?
C32 C31 C30 120.95(14) . . ?
C36 C31 Ca1 84.68(8) . . ?
C36 C31 C30 123.51(13) . . ?
C36 C31 C32 115.43(13) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.58(15) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 119.4 . . ?
C32 C33 C34 121.25(15) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 H34 120.6 . . ?
C35 C34 C33 118.83(14) . . ?
C35 C34 H34 120.6 . . ?
C34 C35 H35 119.5 . . ?
C34 C35 C36 121.00(15) . . ?
C36 C35 H35 119.5 . . ?
Ca1 C36 H36 81.4 . . ?
C31 C36 Ca1 65.62(7) . . ?
C31 C36 H36 119.2 . . ?
C35 C36 Ca1 123.94(10) . . ?
C35 C36 C31 121.51(14) . . ?
C35 C36 H36 119.2 . . ?
C44 C43 H43 120.0 . . ?
C48 C43 H43 120.0 . . ?
C48 C43 C44 120.08(17) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 C43 119.88(16) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.26(16) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 120.1 . . ?
C45 C46 C47 119.72(17) . . ?
C47 C46 H46 120.1 . . ?
C46 C47 H47 120.0 . . ?
C48 C47 C46 120.01(16) . . ?
C48 C47 H47 120.0 . . ?
C43 C48 C47 120.05(16) . . ?
C43 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C38 C37 H37 119.8 . . ?
C38 C37 C42 120.37(17) . . ?
C42 C37 H37 119.8 . . ?
C37 C38 H38 120.0 . . ?
C37 C38 C39 120.04(17) . . ?
C39 C38 H38 120.0 . . ?
C38 C39 H39 120.1 . . ?
C40 C39 C38 119.79(18) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 H40 120.2 . . ?
C39 C40 C41 119.63(18) . . ?
C41 C40 H40 120.2 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.47(17) . . ?
C42 C41 H41 119.8 . . ?
C37 C42 H42 120.2 . . ?
C41 C42 C37 119.69(17) . . ?
C41 C42 H42 120.2 . . ?

_olex2_date_sample_data_collection 2015-04-20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.772
####################################################################### 
# 
# 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_hasj170608b
_database_code_depnum_ccdc_archive 'CCDC 1560716'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_audit_creation_date             2017-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C74 H118 Ca2 I2 N4 O4'
_chemical_formula_sum            'C74 H118 Ca2 I2 N4 O4'
_chemical_formula_weight         1461.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O I Ca'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      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                   29.2848(9)
_cell_length_b                   29.2848(9)
_cell_length_c                   23.2122(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     17239.8(11)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    22490
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2880
_cell_measurement_theta_min      3.3620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-23 7 27 0.1655
-21 40 7 0.0757
40 -27 1 0.1082
-3 -22 -25 0.0908
16 -36 -16 0.1098
16 -28 -24 0.1384
-27 25 -22 0.1230
-16 35 18 0.0557
-8 -12 28 0.1752
-17 30 -22 0.1127
-16 -5 28 0.1575
37 -4 5 0.1312
35 -7 13 0.1229
33 -9 18 0.1293
25 1 23 0.1180
-25 -2 -22 0.1539
18 18 -16 0.1916
22 15 13 0.1220
20 11 21 0.1100
14 5 29 0.1266
10 0 32 0.1410
-20 -18 13 0.1832
-19 -9 -24 0.1327
-13 -2 -30 0.1078
21 13 18 0.1143
1 16 29 0.1094
4 25 21 0.0946
10 26 -14 0.1743
-5 -24 -22 0.1002
1 35 3 0.1221
2 -34 -13 0.0851
-17 30 23 0.0722
-20 14 -29 0.1112
-13 39 8 0.0787
-7 38 -6 0.1125
-15 40 -7 0.1019
15 -38 -13 0.1091
-21 18 27 0.1288
-26 38 -10 0.1086

_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.17
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-23.0078 7.0004 26.9924 -0.1245 -0.4722 0.8781
-20.9988 39.9871 7.0023 -0.6018 -0.7817 -0.0988
39.9783 -26.9765 0.9916 -0.1763 0.9702 -0.0642
-2.9749 -22.0094 -24.9897 0.9305 0.1831 -0.3473
16.0083 -35.9942 -15.9974 0.7441 0.6551 -0.1366
16.0133 -27.9990 -23.9936 0.6854 0.5722 -0.4517
-26.9697 24.9734 -21.9847 0.2896 -0.7230 -0.6095
-16.0097 34.9952 17.9965 -0.7519 -0.6449 0.2025
-8.0150 -11.9892 27.9886 -0.0007 -0.0152 0.9847
-16.9769 29.9773 -21.9861 -0.0148 -0.6039 -0.7833
-16.0110 -4.9941 27.9902 -0.0044 -0.2261 0.9823
36.9733 -3.9796 4.9915 -0.6961 0.6766 -0.2211
34.9687 -6.9765 12.9882 -0.7114 0.6726 0.0516
32.9664 -8.9748 17.9862 -0.7038 0.6586 0.2319
24.9659 1.0221 22.9858 -0.8506 0.4155 0.3235
-24.9665 -2.0215 -21.9864 0.8580 -0.4051 -0.2841
17.9982 17.9985 -15.9952 -0.5078 0.1222 -0.8531
21.9734 15.0140 12.9914 -0.9563 0.2183 -0.0890
19.9690 11.0173 20.9880 -0.9491 0.2249 0.1966
13.9675 5.0191 28.9853 -0.8202 0.1838 0.5517
9.9685 0.0193 31.9844 -0.6765 0.1672 0.7394
-19.9946 -18.0008 12.9968 0.5917 -0.1561 0.7954
-18.9676 -9.0185 -23.9868 0.9304 -0.2283 -0.3128
-12.9679 -2.0195 -29.9849 0.7487 -0.1980 -0.6277
20.9704 13.0161 17.9893 -0.9678 0.2215 0.0803
0.9739 16.0112 28.9880 -0.8178 -0.1550 0.5525
3.9769 25.0076 20.9914 -0.9566 -0.1969 0.1917
10.0004 25.9943 -13.9943 -0.5643 -0.0994 -0.8153
-4.9756 -24.0087 -21.9907 0.9684 0.1693 -0.2201
0.9913 34.9965 3.0002 -0.8512 -0.3509 -0.3816
2.0145 -33.9997 -12.9963 0.9225 0.3933 0.0706
-17.0122 29.9978 22.9943 -0.6961 -0.6102 0.4104
-19.9668 13.9752 -28.9834 0.5084 -0.4863 -0.7303
-13.0044 38.9915 8.0005 -0.7480 -0.6340 -0.1471
-6.9971 37.9881 -5.9944 -0.6288 -0.5185 -0.5713
-14.9915 39.9836 -6.9926 -0.5050 -0.6767 -0.5359
15.0069 -37.9930 -12.9986 0.7628 0.6585 -0.0203
-21.0108 17.9996 26.9926 -0.4101 -0.5534 0.7147
-25.9819 37.9773 -9.9895 -0.2034 -0.8441 -0.4693

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43023
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.777
_diffrn_reflns_theta_min         2.978
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00  48.00   1.00   55.00    --  -11.17  19.00 -90.00   94
  2  ω    -20.00  24.00   1.00   55.00    --  -11.17 -99.00 -90.00   44
  3  ω    -33.00  60.00   1.00   55.00    --  -11.17  38.00 150.00   93
  4  ω    -44.00   3.00   1.00   55.00    --  -11.17  77.00  30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0192017000
_diffrn_orient_matrix_UB_12      -0.0224792000
_diffrn_orient_matrix_UB_13      -0.0151513000
_diffrn_orient_matrix_UB_21      0.0171845000
_diffrn_orient_matrix_UB_22      -0.0105023000
_diffrn_orient_matrix_UB_23      -0.0001223000
_diffrn_orient_matrix_UB_31      -0.0109474000
_diffrn_orient_matrix_UB_32      -0.0128676000
_diffrn_orient_matrix_UB_33      0.0265359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7640
_reflns_number_total             9623
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         1.626
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9623
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0141P)²+123.1176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0984
_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
 C31-C30 \\sim C30-C29 \\sim C32-C31
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C23(H23), C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C19(H19), C20(H20), C21(H21)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_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
I1 I 0.43242(2) 0.47356(2) 0.55098(2) 0.04352(8) Uani 1 1 d . . . . .
Ca1 Ca 0.45599(3) 0.51557(3) 0.42371(2) 0.03135(14) Uani 1 1 d . . . . .
O1 O 0.36169(10) 0.46272(9) 0.41791(10) 0.0409(6) Uani 1 1 d . . . . .
O2 O 0.45232(11) 0.44454(10) 0.36663(9) 0.0435(6) Uani 1 1 d . . . . .
N1 N 0.46113(10) 0.57102(10) 0.34493(10) 0.0288(5) Uani 1 1 d . . . . .
N2 N 0.46634(9) 0.60308(10) 0.43378(10) 0.0253(5) Uani 1 1 d . . . . .
C00B C 0.45263(11) 0.65348(12) 0.35069(12) 0.0261(6) Uani 1 1 d . . . . .
C1 C 0.46324(14) 0.56607(13) 0.28393(12) 0.0347(7) Uani 1 1 d . . . . .
C2 C 0.41839(17) 0.53063(14) 0.25240(14) 0.0422(8) Uani 1 1 d . . . . .
C3 C 0.4242(2) 0.52123(16) 0.19391(15) 0.0565(12) Uani 1 1 d . . . . .
H3 H 0.394370 0.498196 0.172992 0.068 Uiso 1 1 calc R . . . .
C4 C 0.4722(2) 0.54480(18) 0.16693(16) 0.0673(15) Uani 1 1 d . . . . .
H4 H 0.474999 0.537729 0.128442 0.081 Uiso 1 1 calc R . . . .
C5 C 0.5161(2) 0.57912(17) 0.19786(15) 0.0569(12) Uani 1 1 d . . . . .
H5 H 0.548775 0.595254 0.179717 0.068 Uiso 1 1 calc R . . . .
C6 C 0.51317(16) 0.59057(15) 0.25585(13) 0.0421(9) Uani 1 1 d . . . . .
C7 C 0.56396(16) 0.62663(15) 0.28712(14) 0.0440(9) Uani 1 1 d . . . . .
H7 H 0.554482 0.636364 0.323745 0.053 Uiso 1 1 calc R . . . .
C8 C 0.59463(18) 0.59859(18) 0.30139(15) 0.0545(11) Uani 1 1 d . . . . .
H8A H 0.572846 0.567667 0.323878 0.082 Uiso 1 1 calc GR . . . .
H8B H 0.625657 0.621882 0.322951 0.082 Uiso 1 1 calc GR . . . .
H8C H 0.604678 0.588563 0.266327 0.082 Uiso 1 1 calc GR . . . .
C9 C 0.60038(17) 0.67818(18) 0.25469(19) 0.0607(12) Uani 1 1 d . . . . .
H9A H 0.613460 0.670294 0.220411 0.091 Uiso 1 1 calc GR . . . .
H9B H 0.629458 0.701000 0.279020 0.091 Uiso 1 1 calc GR . . . .
H9C H 0.580918 0.695361 0.244435 0.091 Uiso 1 1 calc GR . . . .
C10 C 0.36418(16) 0.49903(15) 0.27907(16) 0.0466(9) Uani 1 1 d . . . . .
H10 H 0.366122 0.511641 0.318599 0.056 Uiso 1 1 calc R . . . .
C11 C 0.34642(19) 0.43965(16) 0.28193(17) 0.0545(10) Uani 1 1 d . . . . .
H11A H 0.344691 0.426445 0.243662 0.082 Uiso 1 1 calc GR . . . .
H11B H 0.312261 0.420769 0.299599 0.082 Uiso 1 1 calc GR . . . .
H11C H 0.371305 0.434892 0.304309 0.082 Uiso 1 1 calc GR . . . .
C12 C 0.32145(19) 0.50509(17) 0.2470(2) 0.0658(13) Uani 1 1 d . . . . .
H12A H 0.331873 0.541759 0.244657 0.099 Uiso 1 1 calc GR . . . .
H12B H 0.288659 0.486399 0.267429 0.099 Uiso 1 1 calc GR . . . .
H12C H 0.317185 0.490870 0.208801 0.099 Uiso 1 1 calc GR . . . .
C13 C 0.46275(11) 0.60993(11) 0.37712(11) 0.0237(5) Uani 1 1 d . . . . .
C14 C 0.39656(13) 0.62420(13) 0.32637(15) 0.0365(7) Uani 1 1 d . . . . .
H14A H 0.395144 0.602554 0.294586 0.055 Uiso 1 1 calc GR . . . .
H14B H 0.386797 0.649279 0.313416 0.055 Uiso 1 1 calc GR . . . .
H14C H 0.372556 0.602390 0.355863 0.055 Uiso 1 1 calc GR . . . .
C15 C 0.45551(12) 0.69486(11) 0.39333(13) 0.0285(6) Uani 1 1 d . . . . .
H15A H 0.432405 0.677473 0.425253 0.043 Uiso 1 1 calc GR . . . .
H15B H 0.444895 0.717190 0.374344 0.043 Uiso 1 1 calc GR . . . .
H15C H 0.491016 0.715810 0.407072 0.043 Uiso 1 1 calc GR . . . .
C16 C 0.49048(14) 0.68423(14) 0.30087(14) 0.0385(7) Uani 1 1 d . . . . .
H16A H 0.526088 0.702361 0.314905 0.058 Uiso 1 1 calc GR . . . .
H16B H 0.481717 0.709384 0.285696 0.058 Uiso 1 1 calc GR . . . .
H16C H 0.487202 0.660092 0.271009 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.48320(11) 0.64166(12) 0.47811(12) 0.0259(6) Uani 1 1 d . . . . .
C18 C 0.53589(12) 0.68494(14) 0.47958(13) 0.0351(7) Uani 1 1 d . . . . .
C19 C 0.55159(13) 0.72064(14) 0.52517(13) 0.0369(7) Uani 1 1 d . . . . .
H19 H 0.586096 0.748615 0.526186 0.044 Uiso 1 1 calc R . . . .
C20 C 0.51738(13) 0.71564(13) 0.56888(14) 0.0350(7) Uani 1 1 d . . . . .
H20 H 0.528103 0.740784 0.597948 0.042 Uiso 1 1 calc R . . . .
C21 C 0.46695(12) 0.67260(12) 0.56861(12) 0.0295(6) Uani 1 1 d . . . . .
H21 H 0.443983 0.668800 0.598301 0.035 Uiso 1 1 calc R . . . .
C22 C 0.44948(11) 0.63469(11) 0.52514(12) 0.0244(5) Uani 1 1 d . . . . .
C23 C 0.39399(11) 0.58743(11) 0.52874(12) 0.0262(6) Uani 1 1 d . . . . .
H23 H 0.393657 0.559048 0.506044 0.031 Uiso 1 1 calc R . . . .
C24 C 0.37743(14) 0.56651(13) 0.59041(13) 0.0369(7) Uani 1 1 d . . . . .
H24A H 0.404104 0.561003 0.607612 0.055 Uiso 1 1 calc GR . . . .
H24B H 0.344659 0.533740 0.589355 0.055 Uiso 1 1 calc GR . . . .
H24C H 0.373186 0.591719 0.612764 0.055 Uiso 1 1 calc GR . . . .
C25 C 0.35277(12) 0.59875(13) 0.50248(15) 0.0357(7) Uani 1 1 d . . . . .
H25A H 0.353371 0.627783 0.522386 0.054 Uiso 1 1 calc GR . . . .
H25B H 0.318439 0.568082 0.506097 0.054 Uiso 1 1 calc GR . . . .
H25C H 0.360633 0.607498 0.462487 0.054 Uiso 1 1 calc GR . . . .
C26 C 0.57674(13) 0.69305(19) 0.43424(15) 0.0556(11) Uani 1 1 d . . . . .
H26 H 0.558397 0.669674 0.401686 0.067 Uiso 1 1 calc R . . . .
C27 C 0.61566(15) 0.67763(19) 0.45889(19) 0.0612(12) Uani 1 1 d . . . . .
H27A H 0.634605 0.700573 0.490408 0.092 Uiso 1 1 calc GR . . . .
H27B H 0.640086 0.680816 0.429418 0.092 Uiso 1 1 calc GR . . . .
H27C H 0.596694 0.641847 0.472297 0.092 Uiso 1 1 calc GR . . . .
C28 C 0.60743(16) 0.7506(2) 0.4113(2) 0.0806(18) Uani 1 1 d . . . . .
H28A H 0.582871 0.761103 0.398607 0.121 Uiso 1 1 calc GR . . . .
H28B H 0.629361 0.752455 0.379577 0.121 Uiso 1 1 calc GR . . . .
H28C H 0.629036 0.773648 0.441506 0.121 Uiso 1 1 calc GR . . . .
C29 C 0.32594(15) 0.48268(15) 0.42290(17) 0.0472(9) Uani 1 1 d D . . . .
H29A H 0.305229 0.476067 0.388080 0.057 Uiso 1 1 calc R . . . .
H29B H 0.344693 0.520226 0.430839 0.057 Uiso 1 1 calc R . . . .
C30 C 0.29292(18) 0.45299(16) 0.47126(18) 0.0555(10) Uani 1 1 d D . . . .
H30A H 0.260722 0.454743 0.472477 0.067 Uiso 1 1 calc R . . . .
H30B H 0.311494 0.465586 0.507547 0.067 Uiso 1 1 calc R . . . .
C31 C 0.2812(2) 0.39559(16) 0.4575(2) 0.0640(13) Uani 1 1 d D . . . .
H31A H 0.273126 0.374472 0.492187 0.077 Uiso 1 1 calc R . . . .
H31B H 0.252343 0.378004 0.430351 0.077 Uiso 1 1 calc R . . . .
C32 C 0.33275(16) 0.40634(14) 0.43142(16) 0.0445(8) Uani 1 1 d D . . . .
H32A H 0.352458 0.397618 0.458505 0.053 Uiso 1 1 calc R . . . .
H32B H 0.326631 0.385567 0.396744 0.053 Uiso 1 1 calc R . . . .
C33 C 0.44915(17) 0.39669(14) 0.39019(14) 0.0432(8) Uani 1 1 d . . . . .
H33A H 0.413360 0.371938 0.402136 0.052 Uiso 1 1 calc R . . . .
H33B H 0.472271 0.405112 0.423243 0.052 Uiso 1 1 calc R . . . .
C34 C 0.46632(14) 0.37326(14) 0.34195(14) 0.0379(7) Uani 1 1 d . . . . .
H34A H 0.502161 0.380638 0.347937 0.045 Uiso 1 1 calc R . . . .
H34B H 0.443096 0.335407 0.339419 0.045 Uiso 1 1 calc R . . . .
C35 C 0.46243(16) 0.40068(16) 0.28803(15) 0.0464(9) Uani 1 1 d . . . . .
H35A H 0.486360 0.402145 0.258247 0.056 Uiso 1 1 calc R . . . .
H35B H 0.426768 0.383364 0.272930 0.056 Uiso 1 1 calc R . . . .
C36 C 0.47845(19) 0.45457(16) 0.31086(14) 0.0516(10) Uani 1 1 d . . . . .
H36A H 0.516428 0.475480 0.315144 0.062 Uiso 1 1 calc R . . . .
H36B H 0.466718 0.472939 0.285417 0.062 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
I1 Ca1 3.1414(6) . ?
I1 Ca1 3.1755(7) 10_666 ?
Ca1 O1 2.401(3) . ?
Ca1 O2 2.423(2) . ?
Ca1 N1 2.400(2) . ?
Ca1 N2 2.437(2) . ?
O1 C29 1.436(4) . ?
O1 C32 1.464(4) . ?
O2 C33 1.463(4) . ?
O2 C36 1.457(4) . ?
N1 C1 1.428(4) . ?
N1 C13 1.343(4) . ?
N2 C13 1.342(3) . ?
N2 C17 1.422(4) . ?
C00B C13 1.571(4) . ?
C00B C14 1.530(4) . ?
C00B C15 1.534(4) . ?
C00B C16 1.542(4) . ?
C1 C2 1.405(5) . ?
C1 C6 1.424(5) . ?
C2 C3 1.412(5) . ?
C2 C10 1.514(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.369(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.373(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.400(5) . ?
C6 C7 1.511(6) . ?
C7 H7 0.9800 . ?
C7 C8 1.526(5) . ?
C7 C9 1.540(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C11 1.547(5) . ?
C10 C12 1.541(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.426(4) . ?
C17 C22 1.417(4) . ?
C18 C19 1.394(5) . ?
C18 C26 1.520(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.381(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.395(4) . ?
C22 C23 1.521(4) . ?
C23 H23 0.9800 . ?
C23 C24 1.537(4) . ?
C23 C25 1.529(4) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26 0.9800 . ?
C26 C27 1.531(6) . ?
C26 C28 1.554(7) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.453(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.571(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.506(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.524(4) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.522(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.500(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 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
Ca1 I1 Ca1 96.960(15) . 10_666 ?
I1 Ca1 I1 83.042(15) . 10_666 ?
O1 Ca1 I1 81.01(6) . . ?
O1 Ca1 I1 150.37(6) . 10_666 ?
O1 Ca1 O2 82.70(9) . . ?
O1 Ca1 N2 100.45(8) . . ?
O2 Ca1 I1 77.81(6) . 10_666 ?
O2 Ca1 I1 105.74(6) . . ?
O2 Ca1 N2 152.15(8) . . ?
N1 Ca1 I1 155.34(6) . . ?
N1 Ca1 I1 111.09(6) . 10_666 ?
N1 Ca1 O1 93.22(9) . . ?
N1 Ca1 O2 97.19(8) . . ?
N1 Ca1 N2 55.15(8) . . ?
N2 Ca1 I1 102.07(6) . . ?
N2 Ca1 I1 107.23(6) . 10_666 ?
C29 O1 Ca1 124.8(2) . . ?
C29 O1 C32 108.2(3) . . ?
C32 O1 Ca1 123.06(19) . . ?
C33 O2 Ca1 124.90(18) . . ?
C36 O2 Ca1 121.3(2) . . ?
C36 O2 C33 107.5(2) . . ?
C1 N1 Ca1 132.70(18) . . ?
C13 N1 Ca1 96.54(16) . . ?
C13 N1 C1 130.7(2) . . ?
C13 N2 Ca1 94.90(17) . . ?
C13 N2 C17 127.8(2) . . ?
C17 N2 Ca1 135.75(17) . . ?
C14 C00B C13 105.9(2) . . ?
C14 C00B C15 107.5(2) . . ?
C14 C00B C16 107.9(3) . . ?
C15 C00B C13 115.5(2) . . ?
C15 C00B C16 106.4(2) . . ?
C16 C00B C13 113.2(2) . . ?
C2 C1 N1 121.3(3) . . ?
C2 C1 C6 118.6(3) . . ?
C6 C1 N1 119.2(3) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 C10 123.1(3) . . ?
C3 C2 C10 117.8(4) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.4(4) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.6(3) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 122.1(4) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C7 122.4(3) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C7 118.2(4) . . ?
C6 C7 H7 107.3 . . ?
C6 C7 C8 111.5(3) . . ?
C6 C7 C9 114.0(3) . . ?
C8 C7 H7 107.3 . . ?
C8 C7 C9 109.2(3) . . ?
C9 C7 H7 107.3 . . ?
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 . . ?
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 . . ?
C2 C10 H10 107.9 . . ?
C2 C10 C11 111.4(3) . . ?
C2 C10 C12 113.3(3) . . ?
C11 C10 H10 107.9 . . ?
C12 C10 H10 107.9 . . ?
C12 C10 C11 108.3(3) . . ?
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 . . ?
N1 C13 C00B 122.0(2) . . ?
N2 C13 N1 113.0(2) . . ?
N2 C13 C00B 124.4(2) . . ?
C00B C14 H14A 109.5 . . ?
C00B C14 H14B 109.5 . . ?
C00B C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C00B C15 H15A 109.5 . . ?
C00B C15 H15B 109.5 . . ?
C00B C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C00B C16 H16A 109.5 . . ?
C00B C16 H16B 109.5 . . ?
C00B C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C18 121.0(3) . . ?
C22 C17 N2 120.2(3) . . ?
C22 C17 C18 118.4(3) . . ?
C17 C18 C26 122.7(3) . . ?
C19 C18 C17 119.3(3) . . ?
C19 C18 C26 118.0(3) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 C18 121.9(3) . . ?
C20 C19 H19 119.1 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(3) . . ?
C21 C20 H20 120.6 . . ?
C20 C21 H21 119.0 . . ?
C20 C21 C22 121.9(3) . . ?
C22 C21 H21 119.0 . . ?
C17 C22 C23 121.6(3) . . ?
C21 C22 C17 119.4(3) . . ?
C21 C22 C23 119.0(3) . . ?
C22 C23 H23 107.2 . . ?
C22 C23 C24 113.2(2) . . ?
C22 C23 C25 112.4(2) . . ?
C24 C23 H23 107.2 . . ?
C25 C23 H23 107.2 . . ?
C25 C23 C24 109.4(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C18 C26 H26 108.1 . . ?
C18 C26 C27 109.8(3) . . ?
C18 C26 C28 113.0(4) . . ?
C27 C26 H26 108.1 . . ?
C27 C26 C28 109.6(3) . . ?
C28 C26 H26 108.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 H29A 111.2 . . ?
O1 C29 H29B 111.2 . . ?
O1 C29 C30 102.8(3) . . ?
H29A C29 H29B 109.1 . . ?
C30 C29 H29A 111.2 . . ?
C30 C29 H29B 111.2 . . ?
C29 C30 H30A 111.4 . . ?
C29 C30 H30B 111.4 . . ?
C29 C30 C31 101.9(3) . . ?
H30A C30 H30B 109.2 . . ?
C31 C30 H30A 111.4 . . ?
C31 C30 H30B 111.4 . . ?
C30 C31 H31A 111.5 . . ?
C30 C31 H31B 111.5 . . ?
H31A C31 H31B 109.3 . . ?
C32 C31 C30 101.4(3) . . ?
C32 C31 H31A 111.5 . . ?
C32 C31 H31B 111.5 . . ?
O1 C32 C31 106.0(3) . . ?
O1 C32 H32A 110.5 . . ?
O1 C32 H32B 110.5 . . ?
C31 C32 H32A 110.5 . . ?
C31 C32 H32B 110.5 . . ?
H32A C32 H32B 108.7 . . ?
O2 C33 H33A 110.5 . . ?
O2 C33 H33B 110.5 . . ?
O2 C33 C34 106.2(3) . . ?
H33A C33 H33B 108.7 . . ?
C34 C33 H33A 110.5 . . ?
C34 C33 H33B 110.5 . . ?
C33 C34 H34A 111.0 . . ?
C33 C34 H34B 111.0 . . ?
H34A C34 H34B 109.0 . . ?
C35 C34 C33 103.8(2) . . ?
C35 C34 H34A 111.0 . . ?
C35 C34 H34B 111.0 . . ?
C34 C35 H35A 111.5 . . ?
C34 C35 H35B 111.5 . . ?
H35A C35 H35B 109.3 . . ?
C36 C35 C34 101.4(3) . . ?
C36 C35 H35A 111.5 . . ?
C36 C35 H35B 111.5 . . ?
O2 C36 C35 104.2(3) . . ?
O2 C36 H36A 110.9 . . ?
O2 C36 H36B 110.9 . . ?
C35 C36 H36A 110.9 . . ?
C35 C36 H36B 110.9 . . ?
H36A C36 H36B 108.9 . . ?

_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 0.000 0.000 0.000 72.9 0.0 ?
2 0.000 0.000 0.264 16.2 0.4 ?
3 0.000 0.000 0.500 210.7 41.5 ?
4 0.000 0.000 0.736 16.2 0.0 ?
5 0.000 0.500 0.000 55.0 0.0 ?
6 0.167 0.333 0.333 55.0 0.0 ?
7 0.167 0.833 0.333 55.0 0.0 ?
8 0.333 0.667 0.167 210.7 41.5 ?
9 0.333 0.167 0.667 55.0 0.0 ?
10 0.333 0.667 0.667 72.9 0.0 ?
11 0.333 0.667 0.402 16.2 0.0 ?
12 0.333 0.667 0.931 16.2 0.4 ?
13 0.500 1.000 0.000 55.0 0.0 ?
14 0.500 0.500 0.000 55.0 0.0 ?
15 0.667 0.333 0.833 210.7 41.5 ?
16 0.667 0.833 0.333 55.0 0.0 ?
17 0.667 0.333 0.333 72.9 0.0 ?
18 0.667 0.333 0.069 16.2 0.0 ?
19 0.667 0.333 0.598 16.2 0.4 ?
20 0.833 0.667 0.667 55.0 0.0 ?
21 0.833 0.167 0.667 55.0 0.0 ?


_olex2_date_sample_data_collection 2017-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.795
