# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_hasj220112b
_database_code_depnum_ccdc_archive 'CCDC 2427514'
loop_
_audit_author_name
_audit_author_address
'Jens Langer'
;FAU Erlangen
Germany
;
_audit_update_record             
;
2025-02-27 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_audit_creation_date             2025-02-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H134 Ca2 N4 O3, 2(C5 H12)'
_chemical_formula_sum            'C94 H158 Ca2 N4 O3'
_chemical_formula_weight         1472.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         C94H158Ca2N4O3
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'
O O 0.0492 0.0322 '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                   12.7723(3)
_cell_length_b                   12.8615(3)
_cell_length_c                   16.5534(3)
_cell_angle_alpha                71.5478(17)
_cell_angle_beta                 72.2458(17)
_cell_angle_gamma                62.332(2)
_cell_volume                     2243.75(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    18084
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      74.3360
_cell_measurement_theta_min      3.9270
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.700
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             814
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 10 0.1204
0 -2 0 0.1473
-3 5 -4 0.0740
-2 -1 -11 0.0858
-1 6 7 0.1114
-1 0 0 0.0623
-4 -7 2 0.0924
-7 0 -5 0.0691
2 -5 5 0.1565
-1 -1 1 0.0758
7 3 -2 0.1278
-1 0 0 0.0720
-1 -3 8 0.0976
5 -4 -1 0.1496
1 1 1 0.1032
-1 -1 -1 0.0645
5 8 1 0.0858
-5 -8 -2 0.0790
7 7 3 0.0862
1 0 0 0.0675
6 1 -5 0.1179

_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
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
1.8583 0.5157 10.3775 0.1808 0.7522 -0.6336
0.4924 -1.5039 0.0033 -0.0190 -0.1071 -0.2183
-2.5661 5.0002 -3.7235 0.0242 0.1058 0.9941
-1.5885 -1.3700 -10.5965 -0.1991 -0.8292 0.5223
-0.7244 5.7692 7.0405 0.2158 0.9030 0.3715
-0.5011 -0.4991 -0.0006 0.0695 -0.0170 -0.0236
-3.8774 -7.0794 2.1957 0.7035 -0.1676 -0.6906
-7.1523 -0.1825 -4.6224 0.6410 -0.1543 0.7519
2.2683 -4.7764 4.7220 0.0433 -0.0092 -0.9990
-1.0048 -0.9988 0.9972 0.1784 0.0404 -0.1009
7.3455 2.6078 -1.8393 -0.9756 -0.1813 -0.1241
-0.9978 0.0033 -0.0026 0.1138 0.0281 0.0737
-1.2378 -2.9759 8.1742 0.5345 0.4582 -0.7102
4.9505 -3.5057 -1.2577 -0.5284 -0.4507 -0.7195
0.9994 0.9977 0.9997 -0.0997 0.1083 -0.0065
-0.9994 -0.9977 -0.9997 0.0997 -0.1083 0.0065
4.5837 7.9677 0.7642 -0.6904 0.4233 0.5866
-5.4144 -7.9179 -1.6143 0.7508 -0.4601 -0.4738
6.8776 7.3249 3.3525 -0.8354 0.5115 0.2010
0.5011 0.4991 0.0006 -0.0695 0.0170 0.0236
5.5106 1.3664 -5.4672 -0.8772 -0.4769 0.0560

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.394
_diffrn_reflns_theta_min         2.865
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_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 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00 -24.00   1.00    3.00    --  -41.44 -38.00   0.00   86
  2  ω    -68.00  -9.00   1.00    3.00    --  -41.44 125.00 150.00   59
  3  ω    -65.00  17.00   1.00    3.00    --  -41.44  57.00 150.00   82
  4  ω   -115.00 -19.00   1.00    3.00    --  -41.44 -38.00 -90.00   96
  5  ω     53.00  91.00   1.00    3.00    --   41.44-125.00   0.00   38
  6  ω     53.00 106.00   1.00   12.00    --  107.95-111.00-180.00   53
  7  ω    127.00 178.00   1.00   12.00    --  107.95  77.00   0.00   51
  8  ω     72.00 128.00   1.00   12.00    --  107.95 178.00   0.00   56
  9  ω     36.00 109.00   1.00   12.00    --  107.95-111.00 120.00   73
 10  ω     30.00 153.00   1.00   12.00    --  107.95 -15.00 -90.00  123
 11  ω     42.00 109.00   1.00   12.00    --  107.95-111.00 -30.00   67
 12  ω     37.00 106.00   1.00   12.00    --  107.95 -94.00-150.00   69
 13  ω    100.00 176.00   1.00   12.00    --  107.95  45.00  90.00   76
 14  ω     42.00 132.00   1.00   12.00    --  107.95 -61.00 -60.00   90
 15  ω     32.00 123.00   1.00   12.00    --  107.95 -30.00  60.00   91
 16  ω    -87.00  -6.00   1.00    3.00    --  -41.69 125.00 -90.00   81
 17  ω   -114.00 -14.00   1.00    3.00    --  -41.69 -57.00 120.00  100
 18  ω   -114.00 -14.00   1.00    3.00    --  -41.69 -57.00-150.00  100
 19  ω     14.00 115.00   1.00    3.00    --   41.69  57.00  90.00  101
 20  ω     79.00 178.00   1.00   12.00    --  107.95  61.00 -90.00   99
 21  ω     55.00 178.00   1.00   12.00    --  107.95  15.00-120.00  123
 22  ω     82.00 178.00   1.00   12.00    --  107.95  45.00  60.00   96
 23  ω     79.00 178.00   1.00   12.00    --  107.95  61.00   0.00   99
 24  ω     55.00 178.00   1.00   12.00    --  107.95  15.00   0.00  123
 25  ω     79.00 178.00   1.00   12.00    --  107.95  61.00 150.00   99
 26  ω     79.00 178.00   1.00   12.00    --  107.95  61.00-120.00   99
 27  ω     79.00 178.00   1.00   12.00    --  107.95  61.00 120.00   99
 28  ω    -87.00  -6.00   1.00    3.00    --  -41.69 125.00 -30.00   81
 29  ω     14.00  70.00   1.00    3.00    --   41.69  57.00   0.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1142621000
_diffrn_orient_matrix_UB_12      -0.0246681000
_diffrn_orient_matrix_UB_13      0.0391073000
_diffrn_orient_matrix_UB_21      -0.0281121000
_diffrn_orient_matrix_UB_22      0.0621615000
_diffrn_orient_matrix_UB_23      0.0744310000
_diffrn_orient_matrix_UB_31      -0.0733568000
_diffrn_orient_matrix_UB_32      0.1210006000
_diffrn_orient_matrix_UB_33      -0.0539343000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                7915
_reflns_number_total             8939
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8939
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.033
_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)+(0.0590P)²+1.1679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1177
_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
 C52-C51 \\sim C51-C50 \\sim C49-C50 \\sim C49-C48 \\sim C47-C46 \\sim C45-C46
\\sim C45-C44 \\sim C43-C44
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C48, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C43(0.5) H43a(0.5) H43b(0.5) H43c(0.5) C44(0.5) H44a(0.5)
 H44b(0.5) C45(0.5) H45a(0.5) H45b(0.5) C46(0.5) H46a(0.5) H46b(0.5) C47(0.5)
 H47a(0.5) H47b(0.5) H47c(0.5) C48(0.5) H48a(0.5) H48b(0.5) H48c(0.5) C49(0.5)
 H49a(0.5) H49b(0.5) C50(0.5) H50a(0.5) H50b(0.5) C51(0.5) H51a(0.5) H51b(0.5)
 C52(0.5) H52a(0.5) H52b(0.5) H52c(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C15(H15a,H15b), C18(H18a,H18b), C20(H20a,H20b), C29(H29a,
 H29b), C31(H31a,H31b), C34(H34a,H34b), C36(H36a,H36b), C38(H38a,H38b),
 C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C44(H44a,H44b),
  C45(H45a,H45b), C46(H46a,H46b), C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c),
 C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C30(H30a,H30b,H30c), C32(H32a,H32b,
 H32c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C43(H43a,H43b,H43c), C47(H47a,
 H47b,H47c), C48(H48a,H48b,H48c), C52(H52a,H52b,H52c)
;
_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
Ca1 Ca 0.57845(3) 0.50664(3) 0.37162(2) 0.02139(9) Uani 1 1 d . . . . .
O1 O 0.500000 0.500000 0.500000 0.0415(4) Uani 1 2 d S . P . .
O2 O 0.72360(10) 0.59416(10) 0.33240(7) 0.0267(2) Uani 1 1 d . . . . .
N1 N 0.48841(11) 0.60546(11) 0.24316(8) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.69462(11) 0.34818(11) 0.29040(8) 0.0203(3) Uani 1 1 d . . . . .
C1 C 0.51683(15) 0.67352(15) 0.08384(10) 0.0277(3) Uani 1 1 d . . . . .
H1A H 0.446378 0.668240 0.076300 0.042 Uiso 1 1 calc R U . . .
H1B H 0.582097 0.652646 0.034008 0.042 Uiso 1 1 calc R U . . .
H1C H 0.495567 0.755541 0.088046 0.042 Uiso 1 1 calc R U . . .
C2 C 0.55780(14) 0.58695(14) 0.16622(10) 0.0217(3) Uani 1 1 d . . . . .
C3 C 0.67069(14) 0.48969(14) 0.15194(10) 0.0222(3) Uani 1 1 d . . . . .
H3 H 0.7094(17) 0.4960(17) 0.0937(13) 0.027(5) Uiso 1 1 d . . . . .
C4 C 0.72900(13) 0.37864(13) 0.20540(10) 0.0214(3) Uani 1 1 d . . . . .
C5 C 0.84142(15) 0.29220(15) 0.15663(11) 0.0278(3) Uani 1 1 d . . . . .
H5A H 0.910491 0.309504 0.151588 0.042 Uiso 1 1 calc R U . . .
H5B H 0.829113 0.302038 0.098596 0.042 Uiso 1 1 calc R U . . .
H5C H 0.856869 0.209529 0.188396 0.042 Uiso 1 1 calc R U . . .
C6 C 0.37005(13) 0.70052(14) 0.24184(9) 0.0213(3) Uani 1 1 d . . . . .
C7 C 0.27583(14) 0.67596(14) 0.23651(10) 0.0239(3) Uani 1 1 d . . . . .
C8 C 0.16159(14) 0.76920(15) 0.23459(11) 0.0279(3) Uani 1 1 d . . . . .
H8 H 0.097640 0.753414 0.231048 0.033 Uiso 1 1 calc R U . . .
C9 C 0.13919(15) 0.88409(15) 0.23772(11) 0.0289(3) Uani 1 1 d . . . . .
H9 H 0.061033 0.946634 0.235626 0.035 Uiso 1 1 calc R U . . .
C10 C 0.23202(14) 0.90685(14) 0.24393(10) 0.0261(3) Uani 1 1 d . . . . .
H10 H 0.216623 0.985780 0.245940 0.031 Uiso 1 1 calc R U . . .
C11 C 0.34768(14) 0.81662(14) 0.24730(10) 0.0223(3) Uani 1 1 d . . . . .
C12 C 0.44568(14) 0.84242(14) 0.25991(10) 0.0241(3) Uani 1 1 d . . . . .
H12 H 0.524472 0.779902 0.238133 0.029 Uiso 1 1 calc R U . . .
C13 C 0.43940(15) 0.82662(15) 0.35785(11) 0.0277(3) Uani 1 1 d . . . . .
H13A H 0.438747 0.747007 0.388104 0.033 Uiso 1 1 calc R U . . .
H13B H 0.513485 0.826781 0.365038 0.033 Uiso 1 1 calc R U . . .
C14 C 0.33103(15) 0.92168(16) 0.40198(11) 0.0306(4) Uani 1 1 d . . . . .
H14A H 0.335449 0.999884 0.377262 0.046 Uiso 1 1 calc R U . . .
H14B H 0.331043 0.900641 0.464292 0.046 Uiso 1 1 calc R U . . .
H14C H 0.256894 0.925657 0.392787 0.046 Uiso 1 1 calc R U . . .
C15 C 0.44666(16) 0.96464(15) 0.20942(11) 0.0296(3) Uani 1 1 d . . . . .
H15A H 0.367723 1.028457 0.227184 0.036 Uiso 1 1 calc R U . . .
H15B H 0.508818 0.975852 0.225436 0.036 Uiso 1 1 calc R U . . .
C16 C 0.47142(19) 0.97957(18) 0.11152(12) 0.0386(4) Uani 1 1 d . . . . .
H16A H 0.469906 1.059668 0.083693 0.058 Uiso 1 1 calc R U . . .
H16B H 0.409564 0.970039 0.094808 0.058 Uiso 1 1 calc R U . . .
H16C H 0.550736 0.918633 0.092946 0.058 Uiso 1 1 calc R U . . .
C17 C 0.29761(15) 0.54929(15) 0.23605(11) 0.0268(3) Uani 1 1 d . . . . .
H17 H 0.384900 0.508276 0.211442 0.032 Uiso 1 1 calc R U . . .
C18 C 0.22708(16) 0.54311(17) 0.17881(12) 0.0323(4) Uani 1 1 d . . . . .
H18A H 0.242289 0.458251 0.185648 0.039 Uiso 1 1 calc R U . . .
H18B H 0.139957 0.587360 0.199145 0.039 Uiso 1 1 calc R U . . .
C19 C 0.2599(2) 0.5951(2) 0.08302(13) 0.0441(5) Uani 1 1 d . . . . .
H19A H 0.211800 0.588757 0.050111 0.066 Uiso 1 1 calc R U . . .
H19B H 0.345611 0.550354 0.061883 0.066 Uiso 1 1 calc R U . . .
H19C H 0.243500 0.679670 0.075460 0.066 Uiso 1 1 calc R U . . .
C20 C 0.27594(16) 0.47805(16) 0.32974(12) 0.0320(4) Uani 1 1 d . . . . .
H20A H 0.303886 0.392991 0.327543 0.038 Uiso 1 1 calc R U . . .
H20B H 0.326470 0.481116 0.363189 0.038 Uiso 1 1 calc R U . . .
C21 C 0.14630(17) 0.52108(17) 0.37882(12) 0.0348(4) Uani 1 1 d . . . . .
H21A H 0.095577 0.514598 0.348207 0.052 Uiso 1 1 calc R U . . .
H21B H 0.117432 0.604941 0.382363 0.052 Uiso 1 1 calc R U . . .
H21C H 0.142499 0.471364 0.437448 0.052 Uiso 1 1 calc R U . . .
C22 C 0.74910(13) 0.22372(13) 0.33027(9) 0.0203(3) Uani 1 1 d . . . . .
C23 C 0.69386(13) 0.14812(14) 0.33499(9) 0.0213(3) Uani 1 1 d . . . . .
C24 C 0.74812(14) 0.02651(14) 0.37013(10) 0.0243(3) Uani 1 1 d . . . . .
H24 H 0.712144 -0.024873 0.372633 0.029 Uiso 1 1 calc R U . . .
C25 C 0.85368(15) -0.02155(14) 0.40164(10) 0.0266(3) Uani 1 1 d . . . . .
H25 H 0.890592 -0.105234 0.424291 0.032 Uiso 1 1 calc R U . . .
C26 C 0.90474(14) 0.05370(14) 0.39974(10) 0.0254(3) Uani 1 1 d . . . . .
H26 H 0.975913 0.020963 0.422718 0.030 Uiso 1 1 calc R U . . .
C27 C 0.85408(13) 0.17661(14) 0.36483(10) 0.0221(3) Uani 1 1 d . . . . .
C28 C 0.58123(14) 0.19639(14) 0.29700(10) 0.0231(3) Uani 1 1 d . . . . .
H28 H 0.541341 0.285235 0.292639 0.028 Uiso 1 1 calc R U . . .
C29 C 0.61736(15) 0.17308(16) 0.20452(10) 0.0289(3) Uani 1 1 d . . . . .
H29A H 0.686858 0.193896 0.173253 0.035 Uiso 1 1 calc R U . . .
H29B H 0.644026 0.086291 0.208560 0.035 Uiso 1 1 calc R U . . .
C30 C 0.51769(18) 0.24294(18) 0.15154(12) 0.0377(4) Uani 1 1 d . . . . .
H30A H 0.548462 0.225225 0.093304 0.057 Uiso 1 1 calc R U . . .
H30B H 0.490257 0.329110 0.147189 0.057 Uiso 1 1 calc R U . . .
H30C H 0.450190 0.219473 0.180005 0.057 Uiso 1 1 calc R U . . .
C31 C 0.48946(15) 0.14403(15) 0.35316(10) 0.0259(3) Uani 1 1 d . . . . .
H31A H 0.418862 0.180156 0.324808 0.031 Uiso 1 1 calc R U . . .
H31B H 0.526294 0.056625 0.355289 0.031 Uiso 1 1 calc R U . . .
C32 C 0.44601(16) 0.16423(16) 0.44566(11) 0.0315(4) Uani 1 1 d . . . . .
H32A H 0.416159 0.249864 0.444565 0.047 Uiso 1 1 calc R U . . .
H32B H 0.512904 0.118634 0.477247 0.047 Uiso 1 1 calc R U . . .
H32C H 0.380995 0.137185 0.474685 0.047 Uiso 1 1 calc R U . . .
C33 C 0.91658(14) 0.25351(14) 0.36406(10) 0.0240(3) Uani 1 1 d . . . . .
H33 H 0.871373 0.337751 0.334727 0.029 Uiso 1 1 calc R U . . .
C34 C 0.91550(17) 0.25398(15) 0.45699(12) 0.0324(4) Uani 1 1 d . . . . .
H34A H 0.960897 0.170909 0.486197 0.039 Uiso 1 1 calc R U . . .
H34B H 0.957890 0.303096 0.454363 0.039 Uiso 1 1 calc R U . . .
C35 C 0.7905(2) 0.30234(19) 0.51118(12) 0.0405(4) Uani 1 1 d . . . . .
H35A H 0.751269 0.389278 0.490521 0.061 Uiso 1 1 calc R U . . .
H35B H 0.796604 0.285190 0.572029 0.061 Uiso 1 1 calc R U . . .
H35C H 0.742924 0.263838 0.506021 0.061 Uiso 1 1 calc R U . . .
C36 C 1.04663(16) 0.20773(17) 0.31227(14) 0.0375(4) Uani 1 1 d . . . . .
H36A H 1.092547 0.125547 0.342511 0.045 Uiso 1 1 calc R U . . .
H36B H 1.044261 0.202498 0.254506 0.045 Uiso 1 1 calc R U . . .
C37 C 1.11412(17) 0.28496(19) 0.29967(16) 0.0445(5) Uani 1 1 d . . . . .
H37A H 1.193581 0.252268 0.263308 0.067 Uiso 1 1 calc R U . . .
H37B H 1.123726 0.284890 0.356210 0.067 Uiso 1 1 calc R U . . .
H37C H 1.068419 0.367316 0.271398 0.067 Uiso 1 1 calc R U . . .
C38 C 0.79439(17) 0.60722(17) 0.24657(12) 0.0335(4) Uani 1 1 d . . . . .
H38A H 0.758433 0.597662 0.205634 0.040 Uiso 1 1 calc R U . . .
H38B H 0.876788 0.543202 0.246192 0.040 Uiso 1 1 calc R U . . .
C39 C 0.80099(18) 0.72808(18) 0.21672(13) 0.0390(4) Uani 1 1 d . . . . .
H39A H 0.851930 0.733153 0.158242 0.047 Uiso 1 1 calc R U . . .
H39B H 0.719302 0.792062 0.212794 0.047 Uiso 1 1 calc R U . . .
C40 C 0.85269(17) 0.74734(17) 0.27854(13) 0.0379(4) Uani 1 1 d . . . . .
H40A H 0.847575 0.830361 0.261788 0.046 Uiso 1 1 calc R U . . .
H40B H 0.938499 0.691297 0.276070 0.046 Uiso 1 1 calc R U . . .
C41 C 0.78286(17) 0.72599(17) 0.36962(13) 0.0361(4) Uani 1 1 d . . . . .
H41A H 0.823318 0.728267 0.411015 0.043 Uiso 1 1 calc R U . . .
H41B H 0.701056 0.791327 0.374084 0.043 Uiso 1 1 calc R U . . .
C42 C 0.77296(16) 0.60687(16) 0.39421(11) 0.0309(4) Uani 1 1 d . . . . .
H42A H 0.853787 0.541081 0.397927 0.037 Uiso 1 1 calc R U . . .
H42B H 0.721007 0.599907 0.452122 0.037 Uiso 1 1 calc R U . . .
C43 C 0.8338(9) 0.6770(9) -0.0612(6) 0.078(3) Uani 0.5 1 d D . P A -1
H43A H 0.881191 0.696144 -0.118174 0.117 Uiso 0.5 1 calc R U P A -1
H43B H 0.773379 0.751612 -0.042918 0.117 Uiso 0.5 1 calc R U P A -1
H43C H 0.793424 0.630238 -0.064690 0.117 Uiso 0.5 1 calc R U P A -1
C44 C 0.9162(6) 0.6047(6) 0.0041(4) 0.0677(18) Uani 0.5 1 d D . P A -1
H44A H 0.866347 0.591724 0.062142 0.081 Uiso 0.5 1 calc R U P A -1
H44B H 0.957408 0.652469 0.006115 0.081 Uiso 0.5 1 calc R U P A -1
C45 C 1.0106(6) 0.4839(6) -0.0141(4) 0.0571(15) Uani 0.5 1 d D . P A -1
H45A H 0.969512 0.436120 -0.016424 0.069 Uiso 0.5 1 calc R U P A -1
H45B H 1.060908 0.496737 -0.071957 0.069 Uiso 0.5 1 calc R U P A -1
C46 C 1.0916(6) 0.4124(6) 0.0516(3) 0.0655(16) Uani 0.5 1 d D . P A -1
H46A H 1.040893 0.405792 0.110048 0.079 Uiso 0.5 1 calc R U P A -1
H46B H 1.138119 0.456896 0.050085 0.079 Uiso 0.5 1 calc R U P A -1
C47 C 1.1786(9) 0.2876(9) 0.0378(7) 0.079(3) Uani 0.5 1 d D . P A -1
H47A H 1.233329 0.293066 -0.018168 0.118 Uiso 0.5 1 calc R U P A -1
H47B H 1.133692 0.242970 0.038117 0.118 Uiso 0.5 1 calc R U P A -1
H47C H 1.225275 0.245833 0.084403 0.118 Uiso 0.5 1 calc R U P A -1
C48 C 1.2069(7) -0.0037(11) -0.0150(8) 0.073(3) Uani 0.5 1 d D . P B -1
H48A H 1.234348 -0.007465 -0.076517 0.109 Uiso 0.5 1 calc R U P B -1
H48B H 1.235334 -0.085149 0.020468 0.109 Uiso 0.5 1 calc R U P B -1
H48C H 1.239232 0.043656 -0.001898 0.109 Uiso 0.5 1 calc R U P B -1
C49 C 1.0747(5) 0.0529(6) 0.0045(4) 0.0652(13) Uani 0.5 1 d D . P B -1
H49A H 1.047433 0.132203 -0.035225 0.078 Uiso 0.5 1 calc R U P B -1
H49B H 1.048988 0.067075 0.064297 0.078 Uiso 0.5 1 calc R U P B -1
C50 C 1.0123(11) -0.0159(17) -0.003(2) 0.068(3) Uani 0.5 1 d D . P B -1
H50A H 1.040747 -0.095659 0.036451 0.082 Uiso 0.5 1 calc R U P B -1
H50B H 1.037504 -0.029192 -0.062642 0.082 Uiso 0.5 1 calc R U P B -1
C51 C 0.8784(6) 0.0394(7) 0.0180(6) 0.098(2) Uani 0.5 1 d D . P B -1
H51A H 0.853596 0.048413 0.079050 0.118 Uiso 0.5 1 calc R U P B -1
H51B H 0.850540 0.121123 -0.018655 0.118 Uiso 0.5 1 calc R U P B -1
C52 C 0.8135(14) -0.0239(15) 0.0067(10) 0.149(7) Uani 0.5 1 d D . P B -1
H52A H 0.856911 -0.061071 -0.043805 0.223 Uiso 0.5 1 calc R U P B -1
H52B H 0.732082 0.033700 -0.002091 0.223 Uiso 0.5 1 calc R U P B -1
H52C H 0.808707 -0.086045 0.058660 0.223 Uiso 0.5 1 calc R U P B -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
Ca1 O1 2.0478(3) . ?
Ca1 O2 2.4221(11) . ?
Ca1 N1 2.4254(13) . ?
Ca1 N2 2.4232(13) . ?
O2 C38 1.439(2) . ?
O2 C42 1.4375(19) . ?
N1 C2 1.3311(19) . ?
N1 C6 1.4378(19) . ?
N2 C4 1.327(2) . ?
N2 C22 1.4349(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.519(2) . ?
C2 C3 1.416(2) . ?
C3 H3 0.94(2) . ?
C3 C4 1.411(2) . ?
C4 C5 1.526(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.411(2) . ?
C6 C11 1.412(2) . ?
C7 C8 1.395(2) . ?
C7 C17 1.522(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.384(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.385(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(2) . ?
C11 C12 1.520(2) . ?
C12 H12 1.0000 . ?
C12 C13 1.550(2) . ?
C12 C15 1.533(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.524(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.520(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 1.0000 . ?
C17 C18 1.533(2) . ?
C17 C20 1.548(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.524(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.416(2) . ?
C22 C27 1.409(2) . ?
C23 C24 1.389(2) . ?
C23 C28 1.525(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.397(2) . ?
C27 C33 1.528(2) . ?
C28 H28 1.0000 . ?
C28 C29 1.542(2) . ?
C28 C31 1.538(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.522(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.523(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 1.0000 . ?
C33 C34 1.536(2) . ?
C33 C36 1.544(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.516(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.526(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.509(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.506(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.513(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.511(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C44 1.512(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.515(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.506(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.511(9) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C49 1.470(9) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.487(13) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.489(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.483(11) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 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 Ca1 O2 110.74(3) . . ?
O1 Ca1 N1 130.17(3) . . ?
O1 Ca1 N2 130.80(3) . . ?
O2 Ca1 N1 98.04(4) . . ?
O2 Ca1 N2 97.47(4) . . ?
N2 Ca1 N1 81.53(4) . . ?
Ca1 O1 Ca1 180.0 2_666 . ?
C38 O2 Ca1 122.68(9) . . ?
C42 O2 Ca1 123.93(10) . . ?
C42 O2 C38 111.22(12) . . ?
C2 N1 Ca1 118.82(10) . . ?
C2 N1 C6 116.12(13) . . ?
C6 N1 Ca1 124.00(9) . . ?
C4 N2 Ca1 118.28(10) . . ?
C4 N2 C22 117.04(12) . . ?
C22 N2 Ca1 123.42(9) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 120.06(14) . . ?
N1 C2 C3 125.74(14) . . ?
C3 C2 C1 114.19(13) . . ?
C2 C3 H3 113.2(12) . . ?
C4 C3 C2 132.68(14) . . ?
C4 C3 H3 113.5(12) . . ?
N2 C4 C3 125.56(13) . . ?
N2 C4 C5 120.79(14) . . ?
C3 C4 C5 113.65(13) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 119.21(13) . . ?
C7 C6 C11 120.29(14) . . ?
C11 C6 N1 120.49(13) . . ?
C6 C7 C17 120.54(14) . . ?
C8 C7 C6 118.66(14) . . ?
C8 C7 C17 120.76(14) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 C7 121.60(15) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.24(15) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 119.2 . . ?
C9 C10 C11 121.61(15) . . ?
C11 C10 H10 119.2 . . ?
C6 C11 C12 121.01(14) . . ?
C10 C11 C6 118.56(14) . . ?
C10 C11 C12 120.39(14) . . ?
C11 C12 H12 106.9 . . ?
C11 C12 C13 110.13(13) . . ?
C11 C12 C15 114.78(13) . . ?
C13 C12 H12 106.9 . . ?
C15 C12 H12 106.9 . . ?
C15 C12 C13 110.91(13) . . ?
C12 C13 H13A 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 C12 115.32(14) . . ?
C14 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
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 . . ?
C12 C15 H15A 108.7 . . ?
C12 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 C12 114.01(14) . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
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 . . ?
C7 C17 H17 106.6 . . ?
C7 C17 C18 114.50(14) . . ?
C7 C17 C20 110.62(13) . . ?
C18 C17 H17 106.6 . . ?
C18 C17 C20 111.35(14) . . ?
C20 C17 H17 106.6 . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C19 C18 C17 113.46(15) . . ?
C19 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
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 C20 H20A 108.3 . . ?
C17 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 C17 115.87(14) . . ?
C21 C20 H20A 108.3 . . ?
C21 C20 H20B 108.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N2 118.18(13) . . ?
C27 C22 N2 121.71(13) . . ?
C27 C22 C23 120.11(14) . . ?
C22 C23 C28 121.18(14) . . ?
C24 C23 C22 118.92(14) . . ?
C24 C23 C28 119.78(13) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.41(14) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.32(15) . . ?
C26 C25 H25 120.3 . . ?
C25 C26 H26 119.2 . . ?
C25 C26 C27 121.57(15) . . ?
C27 C26 H26 119.2 . . ?
C22 C27 C33 122.93(14) . . ?
C26 C27 C22 118.58(14) . . ?
C26 C27 C33 118.48(14) . . ?
C23 C28 H28 107.8 . . ?
C23 C28 C29 109.58(13) . . ?
C23 C28 C31 113.34(13) . . ?
C29 C28 H28 107.8 . . ?
C31 C28 H28 107.8 . . ?
C31 C28 C29 110.42(12) . . ?
C28 C29 H29A 108.6 . . ?
C28 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C28 114.52(14) . . ?
C30 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
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 . . ?
C28 C31 H31A 108.6 . . ?
C28 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C28 114.65(13) . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C33 H33 108.3 . . ?
C27 C33 C34 110.64(13) . . ?
C27 C33 C36 110.29(13) . . ?
C34 C33 H33 108.3 . . ?
C34 C33 C36 110.81(14) . . ?
C36 C33 H33 108.3 . . ?
C33 C34 H34A 108.7 . . ?
C33 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
C35 C34 C33 114.07(14) . . ?
C35 C34 H34A 108.7 . . ?
C35 C34 H34B 108.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 108.5 . . ?
C33 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C37 C36 C33 114.98(15) . . ?
C37 C36 H36A 108.5 . . ?
C37 C36 H36B 108.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 H38A 109.3 . . ?
O2 C38 H38B 109.3 . . ?
O2 C38 C39 111.63(14) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.3 . . ?
C39 C38 H38B 109.3 . . ?
C38 C39 H39A 109.4 . . ?
C38 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 C38 110.96(16) . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
C39 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
C39 C40 C41 109.31(15) . . ?
H40A C40 H40B 108.3 . . ?
C41 C40 H40A 109.8 . . ?
C41 C40 H40B 109.8 . . ?
C40 C41 H41A 109.2 . . ?
C40 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C42 C41 C40 112.17(15) . . ?
C42 C41 H41A 109.2 . . ?
C42 C41 H41B 109.2 . . ?
O2 C42 C41 111.84(14) . . ?
O2 C42 H42A 109.2 . . ?
O2 C42 H42B 109.2 . . ?
C41 C42 H42A 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
C43 C44 H44A 108.5 . . ?
C43 C44 H44B 108.5 . . ?
C43 C44 C45 114.9(5) . . ?
H44A C44 H44B 107.5 . . ?
C45 C44 H44A 108.5 . . ?
C45 C44 H44B 108.5 . . ?
C44 C45 H45A 108.6 . . ?
C44 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
C46 C45 C44 114.5(4) . . ?
C46 C45 H45A 108.6 . . ?
C46 C45 H45B 108.6 . . ?
C45 C46 H46A 108.6 . . ?
C45 C46 H46B 108.6 . . ?
C45 C46 C47 114.5(5) . . ?
H46A C46 H46B 107.6 . . ?
C47 C46 H46A 108.6 . . ?
C47 C46 H46B 108.6 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
C48 C49 H49A 108.3 . . ?
C48 C49 H49B 108.3 . . ?
C48 C49 C50 115.8(8) . . ?
H49A C49 H49B 107.4 . . ?
C50 C49 H49A 108.3 . . ?
C50 C49 H49B 108.3 . . ?
C49 C50 H50A 108.2 . . ?
C49 C50 H50B 108.2 . . ?
C49 C50 C51 116.5(11) . . ?
H50A C50 H50B 107.3 . . ?
C51 C50 H50A 108.2 . . ?
C51 C50 H50B 108.2 . . ?
C50 C51 H51A 107.9 . . ?
C50 C51 H51B 107.9 . . ?
H51A C51 H51B 107.2 . . ?
C52 C51 C50 117.8(11) . . ?
C52 C51 H51A 107.9 . . ?
C52 C51 H51B 107.9 . . ?
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 . . ?

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
Ca1 O2 C38 C39 136.95(12) . . . . ?
Ca1 O2 C42 C41 -139.19(12) . . . . ?
Ca1 N1 C2 C1 -161.16(11) . . . . ?
Ca1 N1 C2 C3 19.7(2) . . . . ?
Ca1 N1 C6 C7 -106.00(14) . . . . ?
Ca1 N1 C6 C11 72.91(16) . . . . ?
Ca1 N2 C4 C3 -25.49(19) . . . . ?
Ca1 N2 C4 C5 153.35(11) . . . . ?
Ca1 N2 C22 C23 104.29(13) . . . . ?
Ca1 N2 C22 C27 -75.15(16) . . . . ?
O2 C38 C39 C40 57.7(2) . . . . ?
N1 C2 C3 C4 15.1(3) . . . . ?
N1 C6 C7 C8 -179.50(14) . . . . ?
N1 C6 C7 C17 2.6(2) . . . . ?
N1 C6 C11 C10 178.66(13) . . . . ?
N1 C6 C11 C12 -3.6(2) . . . . ?
N2 C22 C23 C24 177.37(13) . . . . ?
N2 C22 C23 C28 1.4(2) . . . . ?
N2 C22 C27 C26 -177.61(13) . . . . ?
N2 C22 C27 C33 1.0(2) . . . . ?
C1 C2 C3 C4 -164.07(16) . . . . ?
C2 N1 C6 C7 85.90(17) . . . . ?
C2 N1 C6 C11 -95.18(17) . . . . ?
C2 C3 C4 N2 -11.5(3) . . . . ?
C2 C3 C4 C5 169.57(16) . . . . ?
C4 N2 C22 C23 -88.76(17) . . . . ?
C4 N2 C22 C27 91.80(17) . . . . ?
C6 N1 C2 C1 7.6(2) . . . . ?
C6 N1 C2 C3 -171.57(14) . . . . ?
C6 C7 C8 C9 0.0(2) . . . . ?
C6 C7 C17 C18 -144.62(15) . . . . ?
C6 C7 C17 C20 88.59(17) . . . . ?
C6 C11 C12 C13 -92.16(17) . . . . ?
C6 C11 C12 C15 141.84(15) . . . . ?
C7 C6 C11 C10 -2.4(2) . . . . ?
C7 C6 C11 C12 175.34(14) . . . . ?
C7 C8 C9 C10 -0.8(3) . . . . ?
C7 C17 C18 C19 62.5(2) . . . . ?
C7 C17 C20 C21 67.47(18) . . . . ?
C8 C7 C17 C18 37.5(2) . . . . ?
C8 C7 C17 C20 -89.28(18) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
C9 C10 C11 C6 1.7(2) . . . . ?
C9 C10 C11 C12 -176.07(15) . . . . ?
C10 C11 C12 C13 85.58(18) . . . . ?
C10 C11 C12 C15 -40.4(2) . . . . ?
C11 C6 C7 C8 1.6(2) . . . . ?
C11 C6 C7 C17 -176.33(14) . . . . ?
C11 C12 C13 C14 -70.08(18) . . . . ?
C11 C12 C15 C16 -63.04(19) . . . . ?
C13 C12 C15 C16 171.36(15) . . . . ?
C15 C12 C13 C14 58.08(18) . . . . ?
C17 C7 C8 C9 177.94(15) . . . . ?
C18 C17 C20 C21 -61.05(19) . . . . ?
C20 C17 C18 C19 -171.08(16) . . . . ?
C22 N2 C4 C3 166.87(14) . . . . ?
C22 N2 C4 C5 -14.3(2) . . . . ?
C22 C23 C24 C25 1.0(2) . . . . ?
C22 C23 C28 C29 95.26(16) . . . . ?
C22 C23 C28 C31 -140.90(14) . . . . ?
C22 C27 C33 C34 117.43(16) . . . . ?
C22 C27 C33 C36 -119.61(17) . . . . ?
C23 C22 C27 C26 3.0(2) . . . . ?
C23 C22 C27 C33 -178.41(13) . . . . ?
C23 C24 C25 C26 1.4(2) . . . . ?
C23 C28 C29 C30 -165.73(14) . . . . ?
C23 C28 C31 C32 57.67(18) . . . . ?
C24 C23 C28 C29 -80.67(17) . . . . ?
C24 C23 C28 C31 43.17(19) . . . . ?
C24 C25 C26 C27 -1.6(2) . . . . ?
C25 C26 C27 C22 -0.6(2) . . . . ?
C25 C26 C27 C33 -179.25(14) . . . . ?
C26 C27 C33 C34 -63.94(18) . . . . ?
C26 C27 C33 C36 59.01(19) . . . . ?
C27 C22 C23 C24 -3.2(2) . . . . ?
C27 C22 C23 C28 -179.14(13) . . . . ?
C27 C33 C34 C35 -59.55(18) . . . . ?
C27 C33 C36 C37 174.39(16) . . . . ?
C28 C23 C24 C25 177.00(14) . . . . ?
C29 C28 C31 C32 -178.96(14) . . . . ?
C31 C28 C29 C30 68.74(18) . . . . ?
C34 C33 C36 C37 -62.8(2) . . . . ?
C36 C33 C34 C35 177.80(15) . . . . ?
C38 O2 C42 C41 57.23(18) . . . . ?
C38 C39 C40 C41 -52.9(2) . . . . ?
C39 C40 C41 C42 51.6(2) . . . . ?
C40 C41 C42 O2 -54.2(2) . . . . ?
C42 O2 C38 C39 -59.23(19) . . . . ?
C43 C44 C45 C46 -179.7(5) . . . . ?
C44 C45 C46 C47 175.0(6) . . . . ?
C48 C49 C50 C51 179.2(16) . . . . ?
C49 C50 C51 C52 176.7(16) . . . . ?

_olex2_date_sample_data_collection 2022-01-12
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.743
_oxdiff_exptl_absorpt_empirical_full_min 0.641
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_hasj211028b
_database_code_depnum_ccdc_archive 'CCDC 2427515'
loop_
_audit_author_name
_audit_author_address
'Jens Langer'
;FAU Erlangen
Germany
;
_audit_update_record             
;
2025-02-27 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_audit_creation_date             2025-02-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H134 Ca2 N4 O4, C6 H14, 1[C6H14]'
_chemical_formula_sum            'C96 H162 Ca2 N4 O4'
_chemical_formula_weight         1516.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         C96Ca2H162N4O4
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'
Ca Ca 0.3641 1.2855 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   12.8220(3)
_cell_length_b                   12.8590(2)
_cell_length_c                   16.6221(3)
_cell_angle_alpha                71.9328(16)
_cell_angle_beta                 71.5933(19)
_cell_angle_gamma                62.498(2)
_cell_volume                     2262.16(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    21002
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      72.6950
_cell_measurement_theta_min      3.9150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             838
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.1647
8 5 3 0.0791
1 1 10 0.0718
7 2 -3 0.0971
8 3 2 0.0939
-8 -3 0 0.1397
-3 0 9 0.0947
0 -5 6 0.1031
-6 -6 2 0.0876
-5 -6 4 0.0862
-2 4 -7 0.1501
-6 1 -6 0.1543
-7 -7 -2 0.0796
-1 -8 1 0.1075
2 -6 2 0.1258
6 -2 0 0.1248
0 -7 -4 0.1386
-8 -7 -4 0.0849
3 8 5 0.1639
-6 -4 -10 0.0874
-1 -3 -11 0.1105
-1 0 -10 0.0775
6 4 -3 0.0865
-1 2 -9 0.1053
-3 4 6 0.1360
8 6 6 0.0749
2 6 9 0.1114

_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.161
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
-0.4990 1.4987 -0.0011 -0.0573 -0.2219 -0.0797
8.1153 5.2525 2.7967 -0.0693 -0.2853 0.9559
0.6550 1.1275 10.4374 0.9725 -0.2328 0.0090
7.0653 2.2875 -2.5101 -0.4503 0.1068 0.8865
8.2532 3.1215 2.3063 -0.0281 0.0056 0.9996
-7.9111 -2.8120 -0.1107 0.2265 -0.0531 -0.9726
-2.7747 -0.2532 8.5050 0.8916 -0.2130 -0.3997
-0.3586 -5.0342 6.0915 0.8235 0.5667 -0.0267
-6.4670 -5.5841 1.9092 0.5240 0.3618 -0.7711
-4.6425 -5.8698 3.7286 0.6891 0.4751 -0.5472
-1.5607 4.2006 -6.5684 -0.8064 -0.5547 -0.2049
-6.3728 0.6333 -5.8925 -0.5153 -0.3535 -0.7807
-7.1636 -6.6841 -1.5425 0.2408 0.5080 -0.8270
-1.4855 -7.5615 0.8087 0.4272 0.8973 -0.1108
2.4411 -5.6396 1.9725 0.4016 0.8423 0.3596
6.1244 -2.0302 -0.4408 -0.0463 0.5957 0.8019
-0.0050 -7.2578 -3.9598 -0.0785 0.9917 0.1020
-7.5659 -6.5684 -4.4068 -0.0411 0.5047 -0.8623
2.5266 8.1000 4.6937 0.0777 -0.9758 0.2045
-5.8861 -4.0614 -9.6337 -0.6898 0.3277 -0.6456
-1.0520 -2.7921 -10.5097 -0.9021 0.4295 -0.0408
-1.0161 -0.4875 -10.3859 -0.9896 0.1296 -0.0621
6.4088 3.7723 -3.4722 -0.5995 -0.1106 0.7927
-0.8889 1.8566 -9.2489 -0.9801 -0.1824 -0.0783
-3.2877 3.6147 6.0863 0.4938 -0.7166 -0.4927
7.7660 5.5238 6.1909 0.2593 -0.3785 0.8886
2.0636 6.3229 8.7462 0.5611 -0.8156 0.1411

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34013
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.684
_diffrn_reflns_theta_min         2.857
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  32.00   1.00    1.00    --  -41.44  57.00 -60.00  102
  2  ω    -74.00  35.00   1.00    1.00    --  -41.44  77.00  60.00  109
  3  ω   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00 150.00  101
  4  ω    103.00 178.00   1.00    3.00    --  104.37  77.00-120.00   75
  5  ω    103.00 178.00   1.00    3.00    --  104.37  77.00-150.00   75
  6  ω    103.00 178.00   1.00    3.00    --  104.37  77.00  30.00   75
  7  ω     32.00 133.00   1.00    3.00    --  104.37 -61.00-120.00  101
  8  ω     31.00 112.00   1.00    3.00    --  104.37-125.00  60.00   81
  9  ω     31.00 130.00   1.00    3.00    --  104.37 -45.00  90.00   99
 10  ω     22.00 106.00   1.00    3.00    --  104.37 -94.00  60.00   84
 11  ω     22.00 106.00   1.00    3.00    --  104.37 -94.00 150.00   84
 12  ω     31.00 112.00   1.00    3.00    --  104.37-125.00 -90.00   81
 13  ω     52.00 178.00   1.00    3.00    --  104.37  15.00   0.00  126
 14  ω   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00-150.00  101
 15  ω   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00  30.00  101
 16  ω   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00 -60.00  101
 17  ω     75.00 177.00   1.00    3.00    --  104.37  61.00-120.00  102
 18  ω     75.00 177.00   1.00    3.00    --  104.37  61.00  60.00  102
 19  ω     75.00 177.00   1.00    3.00    --  104.37  61.00-180.00  102
 20  ω     75.00 177.00   1.00    3.00    --  104.37  61.00  90.00  102
 21  ω     75.00 177.00   1.00    3.00    --  104.37  61.00   0.00  102
 22  ω     75.00 177.00   1.00    3.00    --  104.37  61.00-150.00  102
 23  ω     75.00 177.00   1.00    3.00    --  104.37  61.00  30.00  102
 24  ω     52.00 178.00   1.00    3.00    --  104.37  15.00-180.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147153000
_diffrn_orient_matrix_UB_12      -0.0430415000
_diffrn_orient_matrix_UB_13      0.0987447000
_diffrn_orient_matrix_UB_21      0.0532115000
_diffrn_orient_matrix_UB_22      -0.1303637000
_diffrn_orient_matrix_UB_23      -0.0115645000
_diffrn_orient_matrix_UB_31      0.1268947000
_diffrn_orient_matrix_UB_32      -0.0109045000
_diffrn_orient_matrix_UB_33      -0.0059237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                8412
_reflns_number_total             8804
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.058
_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)+(0.0410P)²+0.6345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0833
_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. Restrained distances
 C44-C45 \\sim C45A-C44A \\sim C43-C44 \\sim C43-C44A \\sim C45A-C45A_$2 \\sim
C45-C45_$2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C44A \\sim C45A: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 4A
4. Others
 Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C44A)=Sof(H44c)=Sof(H44d)=Sof(C45A)=
 Sof(H45c)=Sof(H45d)=1-FVAR(1)
 Sof(H43a)=Sof(H43b)=Sof(H43c)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(C45)=Sof(H45a)=
 Sof(H45b)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C15(H15a,H15b), C18(H18a,H18b), C20(H20a,H20b), C29(H29a,
 H29b), C31(H31a,H31b), C34(H34a,H34b), C36(H36a,H36b), C38(H38a,H38b),
 C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C44(H44a,H44b),
  C45(H45a,H45b), C44A(H44c,H44d), C45A(H45c,H45d)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c),
 C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C30(H30a,H30b,H30c), C32(H32a,H32b,
 H32c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C43(H43a,H43b,H43c), C43(H43d,
 H43e,H43f)
;
_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
Ca1 Ca 0.50711(2) 0.57755(2) 0.37133(2) 0.01566(6) Uani 1 1 d . . . . .
O1 O 0.45001(7) 0.48052(7) 0.49869(5) 0.02363(17) Uani 1 1 d . . . . .
O2 O 0.59447(7) 0.72330(7) 0.33038(5) 0.02020(16) Uani 1 1 d . . . . .
N1 N 0.60645(8) 0.49246(7) 0.24328(6) 0.01580(17) Uani 1 1 d . . . . .
N2 N 0.35011(8) 0.69612(7) 0.29041(6) 0.01524(17) Uani 1 1 d . . . . .
C1 C 0.67160(10) 0.51831(10) 0.08438(7) 0.0226(2) Uani 1 1 d . . . . .
H1A H 0.753826 0.499923 0.086852 0.034 Uiso 1 1 calc R U . . .
H1B H 0.648577 0.581580 0.034070 0.034 Uiso 1 1 calc R U . . .
H1C H 0.667373 0.446444 0.079381 0.034 Uiso 1 1 calc R U . . .
C2 C 0.58632(9) 0.56014(9) 0.16630(7) 0.0167(2) Uani 1 1 d . . . . .
C3 C 0.48910(10) 0.67193(9) 0.15144(7) 0.0175(2) Uani 1 1 d . . . . .
H3 H 0.4944(12) 0.7127(12) 0.0917(9) 0.022(3) Uiso 1 1 d . . . . .
C4 C 0.37922(9) 0.73036(9) 0.20533(7) 0.0162(2) Uani 1 1 d . . . . .
C5 C 0.29247(10) 0.84299(9) 0.15746(7) 0.0215(2) Uani 1 1 d . . . . .
H5A H 0.209668 0.853837 0.186392 0.032 Uiso 1 1 calc R U . . .
H5B H 0.306568 0.835159 0.097726 0.032 Uiso 1 1 calc R U . . .
H5C H 0.305420 0.912364 0.157476 0.032 Uiso 1 1 calc R U . . .
C6 C 0.70159(10) 0.37488(9) 0.24320(6) 0.0166(2) Uani 1 1 d . . . . .
C7 C 0.81766(10) 0.35343(9) 0.24847(6) 0.0171(2) Uani 1 1 d . . . . .
C8 C 0.90808(10) 0.23831(10) 0.24656(7) 0.0207(2) Uani 1 1 d . . . . .
H8 H 0.987180 0.223581 0.248235 0.025 Uiso 1 1 calc R U . . .
C9 C 0.88485(11) 0.14547(10) 0.24227(7) 0.0238(2) Uani 1 1 d . . . . .
H9 H 0.947333 0.067808 0.241239 0.029 Uiso 1 1 calc R U . . .
C10 C 0.76978(11) 0.16670(10) 0.23949(7) 0.0231(2) Uani 1 1 d . . . . .
H10 H 0.753772 0.102466 0.237566 0.028 Uiso 1 1 calc R U . . .
C11 C 0.67685(10) 0.28022(9) 0.23945(7) 0.0192(2) Uani 1 1 d . . . . .
C12 C 0.84446(9) 0.45090(9) 0.26014(7) 0.0180(2) Uani 1 1 d . . . . .
H12 H 0.780464 0.529152 0.239990 0.022 Uiso 1 1 calc R U . . .
C13 C 0.83417(10) 0.44244(9) 0.35698(7) 0.0205(2) Uani 1 1 d . . . . .
H13A H 0.838674 0.514299 0.363194 0.025 Uiso 1 1 calc R U . . .
H13B H 0.753918 0.444278 0.388725 0.025 Uiso 1 1 calc R U . . .
C14 C 0.92891(11) 0.33202(10) 0.39999(7) 0.0234(2) Uani 1 1 d . . . . .
H14A H 1.008618 0.332195 0.372368 0.035 Uiso 1 1 calc R U . . .
H14B H 0.926552 0.259882 0.393709 0.035 Uiso 1 1 calc R U . . .
H14C H 0.912417 0.333077 0.461528 0.035 Uiso 1 1 calc R U . . .
C15 C 0.96538(10) 0.45400(10) 0.20714(7) 0.0226(2) Uani 1 1 d . . . . .
H15A H 0.977475 0.515837 0.222165 0.027 Uiso 1 1 calc R U . . .
H15B H 1.030503 0.375889 0.223581 0.027 Uiso 1 1 calc R U . . .
C16 C 0.97553(12) 0.48024(13) 0.10984(8) 0.0318(3) Uani 1 1 d . . . . .
H16A H 1.053017 0.484794 0.080135 0.048 Uiso 1 1 calc R U . . .
H16B H 0.910318 0.556586 0.093019 0.048 Uiso 1 1 calc R U . . .
H16C H 0.969785 0.416222 0.093699 0.048 Uiso 1 1 calc R U . . .
C17 C 0.55038(10) 0.30086(10) 0.23853(7) 0.0225(2) Uani 1 1 d . . . . .
H17 H 0.509139 0.387490 0.213639 0.027 Uiso 1 1 calc R U . . .
C18 C 0.47884(11) 0.27868(11) 0.33148(8) 0.0262(2) Uani 1 1 d . . . . .
H18A H 0.480545 0.329717 0.364628 0.031 Uiso 1 1 calc R U . . .
H18B H 0.394045 0.305015 0.328769 0.031 Uiso 1 1 calc R U . . .
C19 C 0.52289(12) 0.14979(11) 0.38134(8) 0.0286(3) Uani 1 1 d . . . . .
H19A H 0.517981 0.098471 0.350926 0.043 Uiso 1 1 calc R U . . .
H19B H 0.472564 0.145600 0.439520 0.043 Uiso 1 1 calc R U . . .
H19C H 0.606416 0.122590 0.385558 0.043 Uiso 1 1 calc R U . . .
C20 C 0.54545(12) 0.23033(11) 0.18131(8) 0.0276(3) Uani 1 1 d . . . . .
H20A H 0.589792 0.143901 0.202102 0.033 Uiso 1 1 calc R U . . .
H20B H 0.460700 0.244783 0.187592 0.033 Uiso 1 1 calc R U . . .
C21 C 0.59828(15) 0.26305(15) 0.08574(9) 0.0419(3) Uani 1 1 d . . . . .
H21A H 0.593646 0.213973 0.053225 0.063 Uiso 1 1 calc R U . . .
H21B H 0.682430 0.248460 0.078767 0.063 Uiso 1 1 calc R U . . .
H21C H 0.552689 0.347726 0.063866 0.063 Uiso 1 1 calc R U . . .
C22 C 0.22567(9) 0.74899(9) 0.33019(6) 0.0159(2) Uani 1 1 d . . . . .
C23 C 0.17817(10) 0.85239(9) 0.36553(7) 0.0171(2) Uani 1 1 d . . . . .
C24 C 0.05512(10) 0.90198(9) 0.39973(7) 0.0202(2) Uani 1 1 d . . . . .
H24 H 0.022278 0.971883 0.423238 0.024 Uiso 1 1 calc R U . . .
C25 C -0.02030(10) 0.85187(10) 0.40025(7) 0.0218(2) Uani 1 1 d . . . . .
H25 H -0.104179 0.888364 0.422218 0.026 Uiso 1 1 calc R U . . .
C26 C 0.02804(10) 0.74774(10) 0.36831(7) 0.0201(2) Uani 1 1 d . . . . .
H26 H -0.023366 0.712191 0.370030 0.024 Uiso 1 1 calc R U . . .
C27 C 0.15013(10) 0.69425(9) 0.33383(6) 0.0171(2) Uani 1 1 d . . . . .
C28 C 0.25484(9) 0.91300(9) 0.36773(7) 0.0180(2) Uani 1 1 d . . . . .
H28 H 0.339171 0.869373 0.338216 0.022 Uiso 1 1 calc R U . . .
C29 C 0.25524(10) 0.90584(10) 0.46190(7) 0.0216(2) Uani 1 1 d . . . . .
H29A H 0.304028 0.947249 0.461697 0.026 Uiso 1 1 calc R U . . .
H29B H 0.172013 0.948875 0.491612 0.026 Uiso 1 1 calc R U . . .
C30 C 0.30452(11) 0.77884(11) 0.51294(7) 0.0257(2) Uani 1 1 d . . . . .
H30A H 0.391625 0.741391 0.492352 0.038 Uiso 1 1 calc R U . . .
H30B H 0.266707 0.732708 0.504909 0.038 Uiso 1 1 calc R U . . .
H30C H 0.287009 0.780565 0.574434 0.038 Uiso 1 1 calc R U . . .
C31 C 0.20962(11) 1.04408(10) 0.31870(8) 0.0246(2) Uani 1 1 d . . . . .
H31A H 0.206916 1.045205 0.259552 0.030 Uiso 1 1 calc R U . . .
H31B H 0.126452 1.087859 0.348101 0.030 Uiso 1 1 calc R U . . .
C32 C 0.28547(12) 1.11060(11) 0.31197(9) 0.0302(3) Uani 1 1 d . . . . .
H32A H 0.255841 1.189577 0.274778 0.045 Uiso 1 1 calc R U . . .
H32B H 0.369445 1.064947 0.287121 0.045 Uiso 1 1 calc R U . . .
H32C H 0.279812 1.119994 0.369699 0.045 Uiso 1 1 calc R U . . .
C33 C 0.19884(10) 0.58239(9) 0.29628(7) 0.0188(2) Uani 1 1 d . . . . .
H33 H 0.287740 0.543259 0.292270 0.023 Uiso 1 1 calc R U . . .
C34 C 0.14656(10) 0.49075(10) 0.35284(7) 0.0212(2) Uani 1 1 d . . . . .
H34A H 0.059106 0.526811 0.354714 0.025 Uiso 1 1 calc R U . . .
H34B H 0.182927 0.420493 0.325077 0.025 Uiso 1 1 calc R U . . .
C35 C 0.16659(12) 0.44798(11) 0.44530(7) 0.0270(2) Uani 1 1 d . . . . .
H35A H 0.251901 0.421110 0.444464 0.041 Uiso 1 1 calc R U . . .
H35B H 0.141888 0.381504 0.474043 0.041 Uiso 1 1 calc R U . . .
H35C H 0.118854 0.513835 0.476831 0.041 Uiso 1 1 calc R U . . .
C36 C 0.17599(11) 0.61810(11) 0.20390(7) 0.0243(2) Uani 1 1 d . . . . .
H36A H 0.089049 0.644970 0.207589 0.029 Uiso 1 1 calc R U . . .
H36B H 0.197595 0.686852 0.172376 0.029 Uiso 1 1 calc R U . . .
C37 C 0.24535(13) 0.51883(13) 0.15176(8) 0.0333(3) Uani 1 1 d . . . . .
H37A H 0.226552 0.548919 0.093963 0.050 Uiso 1 1 calc R U . . .
H37B H 0.222366 0.451355 0.181111 0.050 Uiso 1 1 calc R U . . .
H37C H 0.331731 0.492369 0.146691 0.050 Uiso 1 1 calc R U . . .
C38 C 0.60637(11) 0.79474(10) 0.24450(7) 0.0249(2) Uani 1 1 d . . . . .
H38A H 0.541422 0.875949 0.244119 0.030 Uiso 1 1 calc R U . . .
H38B H 0.597475 0.758607 0.203775 0.030 Uiso 1 1 calc R U . . .
C39 C 0.72668(12) 0.80374(11) 0.21460(8) 0.0286(3) Uani 1 1 d . . . . .
H39A H 0.731092 0.855122 0.156363 0.034 Uiso 1 1 calc R U . . .
H39B H 0.791721 0.723318 0.210700 0.034 Uiso 1 1 calc R U . . .
C40 C 0.74397(11) 0.85623(10) 0.27742(8) 0.0279(3) Uani 1 1 d . . . . .
H40A H 0.686306 0.940789 0.275151 0.034 Uiso 1 1 calc R U . . .
H40B H 0.826298 0.853560 0.260875 0.034 Uiso 1 1 calc R U . . .
C41 C 0.72397(11) 0.78488(11) 0.36874(8) 0.0264(2) Uani 1 1 d . . . . .
H41A H 0.790188 0.704261 0.373084 0.032 Uiso 1 1 calc R U . . .
H41B H 0.725302 0.825113 0.410216 0.032 Uiso 1 1 calc R U . . .
C42 C 0.60544(11) 0.77301(10) 0.39248(7) 0.0237(2) Uani 1 1 d . . . . .
H42A H 0.598469 0.720965 0.450241 0.028 Uiso 1 1 calc R U . . .
H42B H 0.538847 0.852738 0.395822 0.028 Uiso 1 1 calc R U . . .
C43 C 0.74293(19) 0.79114(17) -0.07091(12) 0.0619(5) Uani 1 1 d D U . . .
H43A H 0.795405 0.832716 -0.082796 0.093 Uiso 0.944(3) 1 calc R U P A 1
H43B H 0.768439 0.744975 -0.115908 0.093 Uiso 0.944(3) 1 calc R U P A 1
H43C H 0.748013 0.737027 -0.014468 0.093 Uiso 0.944(3) 1 calc R U P A 1
H43D H 0.707611 0.805896 -0.119851 0.093 Uiso 0.056(3) 1 calc R U P A 2
H43E H 0.764170 0.707460 -0.041220 0.093 Uiso 0.056(3) 1 calc R U P A 2
H43F H 0.815289 0.807737 -0.092022 0.093 Uiso 0.056(3) 1 calc R U P A 2
C44 C 0.61553(15) 0.88115(14) -0.07023(10) 0.0406(4) Uani 0.944(3) 1 d D U P A
1
H44A H 0.564985 0.839036 -0.064987 0.049 Uiso 0.944(3) 1 calc R U P A 1
H44B H 0.612456 0.938196 -0.126272 0.049 Uiso 0.944(3) 1 calc R U P A 1
C45 C 0.56233(14) 0.95120(13) 0.00230(10) 0.0332(4) Uani 0.944(3) 1 d D U P A 1
H45A H 0.558578 0.895068 0.058443 0.040 Uiso 0.944(3) 1 calc R U P A 1
H45B H 0.616450 0.987769 0.000212 0.040 Uiso 0.944(3) 1 calc R U P A 1
C44A C 0.655(2) 0.8704(19) -0.0098(14) 0.045(6) Uani 0.056(3) 1 d D U P A 2
H44C H 0.694022 0.915100 -0.000602 0.055 Uiso 0.056(3) 1 calc R U P A 2
H44D H 0.637889 0.818663 0.046376 0.055 Uiso 0.056(3) 1 calc R U P A 2
C45A C 0.536(2) 0.9596(18) -0.0326(13) 0.039(5) Uani 0.056(3) 1 d D U P A 2
H45C H 0.489746 0.916818 -0.034542 0.047 Uiso 0.056(3) 1 calc R U P A 2
H45D H 0.549956 1.008686 -0.090749 0.047 Uiso 0.056(3) 1 calc R U P A 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
Ca1 O1 2.1911(8) . ?
Ca1 O1 2.2131(8) 2_666 ?
Ca1 O2 2.4282(8) . ?
Ca1 N1 2.4074(9) . ?
Ca1 N2 2.4063(9) . ?
O1 O1 1.5932(16) 2_666 ?
O2 C38 1.4434(13) . ?
O2 C42 1.4415(13) . ?
N1 C2 1.3310(14) . ?
N1 C6 1.4391(13) . ?
N2 C4 1.3287(14) . ?
N2 C22 1.4338(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.5199(14) . ?
C2 C3 1.4145(15) . ?
C3 H3 0.966(14) . ?
C3 C4 1.4123(15) . ?
C4 C5 1.5246(14) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.4095(15) . ?
C6 C11 1.4149(15) . ?
C7 C8 1.3990(15) . ?
C7 C12 1.5222(14) . ?
C8 H8 0.9500 . ?
C8 C9 1.3833(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.3846(17) . ?
C10 H10 0.9500 . ?
C10 C11 1.3943(16) . ?
C11 C17 1.5218(16) . ?
C12 H12 1.0000 . ?
C12 C13 1.5463(15) . ?
C12 C15 1.5344(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.5260(15) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.5218(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 1.0000 . ?
C17 C18 1.5437(17) . ?
C17 C20 1.5355(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.5270(17) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5258(18) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.4122(14) . ?
C22 C27 1.4156(15) . ?
C23 C24 1.3959(15) . ?
C23 C28 1.5241(15) . ?
C24 H24 0.9500 . ?
C24 C25 1.3845(16) . ?
C25 H25 0.9500 . ?
C25 C26 1.3877(16) . ?
C26 H26 0.9500 . ?
C26 C27 1.3912(15) . ?
C27 C33 1.5263(14) . ?
C28 H28 1.0000 . ?
C28 C29 1.5408(15) . ?
C28 C31 1.5445(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.5206(16) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5266(16) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 1.0000 . ?
C33 C34 1.5383(15) . ?
C33 C36 1.5418(15) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.5249(16) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.5240(17) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.5117(17) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.5220(18) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.5229(17) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.5123(17) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 H43D 0.9800 . ?
C43 H43E 0.9800 . ?
C43 H43F 0.9800 . ?
C43 C44 1.503(3) . ?
C43 C44A 1.484(14) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.522(2) . ?
C45 C45 1.517(3) 2_675 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C44A H44C 0.9900 . ?
C44A H44D 0.9900 . ?
C44A C45A 1.503(15) . ?
C45A C45A 1.512(16) 2_675 ?
C45A H45C 0.9900 . ?
C45A H45D 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
O1 Ca1 O1 42.41(4) . 2_666 ?
O1 Ca1 O2 91.13(3) 2_666 . ?
O1 Ca1 O2 130.83(3) . . ?
O1 Ca1 N1 124.51(3) . . ?
O1 Ca1 N1 131.63(3) 2_666 . ?
O1 Ca1 N2 144.66(3) 2_666 . ?
O1 Ca1 N2 114.00(3) . . ?
N1 Ca1 O2 96.60(3) . . ?
N2 Ca1 O2 95.72(3) . . ?
N2 Ca1 N1 81.99(3) . . ?
Ca1 O1 Ca1 137.59(4) . 2_666 ?
O1 O1 Ca1 69.53(5) 2_666 . ?
O1 O1 Ca1 68.06(5) 2_666 2_666 ?
C38 O2 Ca1 123.03(6) . . ?
C42 O2 Ca1 122.97(6) . . ?
C42 O2 C38 111.50(8) . . ?
C2 N1 Ca1 120.03(7) . . ?
C2 N1 C6 116.40(8) . . ?
C6 N1 Ca1 122.93(6) . . ?
C4 N2 Ca1 119.28(7) . . ?
C4 N2 C22 116.71(8) . . ?
C22 N2 Ca1 123.22(6) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 119.98(9) . . ?
N1 C2 C3 125.87(10) . . ?
C3 C2 C1 114.15(9) . . ?
C2 C3 H3 114.2(8) . . ?
C4 C3 C2 132.38(10) . . ?
C4 C3 H3 113.0(8) . . ?
N2 C4 C3 125.56(9) . . ?
N2 C4 C5 120.57(9) . . ?
C3 C4 C5 113.85(9) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 120.52(9) . . ?
C7 C6 C11 120.21(9) . . ?
C11 C6 N1 119.26(9) . . ?
C6 C7 C12 121.41(9) . . ?
C8 C7 C6 118.65(10) . . ?
C8 C7 C12 119.87(10) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.46(11) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.44(10) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.49(10) . . ?
C11 C10 H10 119.3 . . ?
C6 C11 C17 120.69(9) . . ?
C10 C11 C6 118.70(10) . . ?
C10 C11 C17 120.58(10) . . ?
C7 C12 H12 106.9 . . ?
C7 C12 C13 110.46(8) . . ?
C7 C12 C15 114.67(9) . . ?
C13 C12 H12 106.9 . . ?
C15 C12 H12 106.9 . . ?
C15 C12 C13 110.55(9) . . ?
C12 C13 H13A 108.3 . . ?
C12 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 C12 115.75(9) . . ?
C14 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
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 . . ?
C12 C15 H15A 108.8 . . ?
C12 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C12 113.84(10) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
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 . . ?
C11 C17 H17 106.6 . . ?
C11 C17 C18 110.73(9) . . ?
C11 C17 C20 114.29(10) . . ?
C18 C17 H17 106.6 . . ?
C20 C17 H17 106.6 . . ?
C20 C17 C18 111.43(9) . . ?
C17 C18 H18A 108.3 . . ?
C17 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C19 C18 C17 115.93(10) . . ?
C19 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
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 C20 H20A 108.8 . . ?
C17 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C17 113.69(10) . . ?
C21 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N2 121.79(9) . . ?
C23 C22 C27 120.08(10) . . ?
C27 C22 N2 118.13(9) . . ?
C22 C23 C28 123.11(9) . . ?
C24 C23 C22 118.58(10) . . ?
C24 C23 C28 118.31(9) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.67(10) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.25(10) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.45(10) . . ?
C27 C26 H26 119.3 . . ?
C22 C27 C33 121.29(9) . . ?
C26 C27 C22 118.86(10) . . ?
C26 C27 C33 119.76(10) . . ?
C23 C28 H28 108.3 . . ?
C23 C28 C29 110.28(9) . . ?
C23 C28 C31 110.72(9) . . ?
C29 C28 H28 108.3 . . ?
C29 C28 C31 110.97(9) . . ?
C31 C28 H28 108.3 . . ?
C28 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 C28 113.85(9) . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
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 . . ?
C28 C31 H31A 108.5 . . ?
C28 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 C28 114.90(10) . . ?
C32 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C33 H33 107.7 . . ?
C27 C33 C34 113.10(9) . . ?
C27 C33 C36 109.69(9) . . ?
C34 C33 H33 107.7 . . ?
C34 C33 C36 110.69(9) . . ?
C36 C33 H33 107.7 . . ?
C33 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C35 C34 C33 114.70(9) . . ?
C35 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 108.6 . . ?
C33 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
C37 C36 C33 114.62(10) . . ?
C37 C36 H36A 108.6 . . ?
C37 C36 H36B 108.6 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 H38A 109.3 . . ?
O2 C38 H38B 109.3 . . ?
O2 C38 C39 111.56(9) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.3 . . ?
C39 C38 H38B 109.3 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
C38 C39 C40 110.38(10) . . ?
H39A C39 H39B 108.1 . . ?
C40 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
C39 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
C39 C40 C41 109.59(9) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.8 . . ?
C41 C40 H40B 109.8 . . ?
C40 C41 H41A 109.3 . . ?
C40 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
C42 C41 C40 111.56(10) . . ?
C42 C41 H41A 109.3 . . ?
C42 C41 H41B 109.3 . . ?
O2 C42 C41 111.84(9) . . ?
O2 C42 H42A 109.2 . . ?
O2 C42 H42B 109.2 . . ?
C41 C42 H42A 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
H43D C43 H43E 109.5 . . ?
H43D C43 H43F 109.5 . . ?
H43E C43 H43F 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
C44A C43 H43D 109.5 . . ?
C44A C43 H43E 109.5 . . ?
C44A C43 H43F 109.5 . . ?
C43 C44 H44A 108.7 . . ?
C43 C44 H44B 108.7 . . ?
C43 C44 C45 114.21(15) . . ?
H44A C44 H44B 107.6 . . ?
C45 C44 H44A 108.7 . . ?
C45 C44 H44B 108.7 . . ?
C44 C45 H45A 108.8 . . ?
C44 C45 H45B 108.8 . . ?
C45 C45 C44 113.61(17) 2_675 . ?
C45 C45 H45A 108.8 2_675 . ?
C45 C45 H45B 108.8 2_675 . ?
H45A C45 H45B 107.7 . . ?
C43 C44A H44C 107.6 . . ?
C43 C44A H44D 107.6 . . ?
C43 C44A C45A 118.9(16) . . ?
H44C C44A H44D 107.0 . . ?
C45A C44A H44C 107.6 . . ?
C45A C44A H44D 107.6 . . ?
C44A C45A H45C 109.4 . . ?
C44A C45A H45D 109.4 . . ?
C45A C45A H45C 109.4 2_675 . ?
C45A C45A H45D 109.4 2_675 . ?
H45C C45A H45D 108.0 . . ?

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
Ca1 O2 C38 C39 -137.85(8) . . . . ?
Ca1 O2 C42 C41 139.67(8) . . . . ?
Ca1 N1 C2 C1 163.47(8) . . . . ?
Ca1 N1 C2 C3 -17.00(14) . . . . ?
Ca1 N1 C6 C7 -74.57(11) . . . . ?
Ca1 N1 C6 C11 104.21(10) . . . . ?
Ca1 N2 C4 C3 24.62(13) . . . . ?
Ca1 N2 C4 C5 -153.88(8) . . . . ?
Ca1 N2 C22 C23 76.26(11) . . . . ?
Ca1 N2 C22 C27 -103.41(9) . . . . ?
O2 C38 C39 C40 -57.58(13) . . . . ?
N1 C2 C3 C4 -14.98(19) . . . . ?
N1 C6 C7 C8 -178.81(9) . . . . ?
N1 C6 C7 C12 3.94(15) . . . . ?
N1 C6 C11 C10 -179.95(9) . . . . ?
N1 C6 C11 C17 -2.03(15) . . . . ?
N2 C22 C23 C24 177.14(9) . . . . ?
N2 C22 C23 C28 -2.54(15) . . . . ?
N2 C22 C27 C26 -176.83(9) . . . . ?
N2 C22 C27 C33 -0.27(14) . . . . ?
C1 C2 C3 C4 164.58(11) . . . . ?
C2 N1 C6 C7 96.23(12) . . . . ?
C2 N1 C6 C11 -84.99(12) . . . . ?
C2 C3 C4 N2 10.26(19) . . . . ?
C2 C3 C4 C5 -171.15(11) . . . . ?
C4 N2 C22 C23 -93.41(12) . . . . ?
C4 N2 C22 C27 86.91(11) . . . . ?
C6 N1 C2 C1 -7.61(14) . . . . ?
C6 N1 C2 C3 171.92(10) . . . . ?
C6 C7 C8 C9 -1.97(16) . . . . ?
C6 C7 C12 C13 94.34(11) . . . . ?
C6 C7 C12 C15 -139.95(10) . . . . ?
C6 C11 C17 C18 -89.69(12) . . . . ?
C6 C11 C17 C20 143.49(10) . . . . ?
C7 C6 C11 C10 -1.16(15) . . . . ?
C7 C6 C11 C17 176.75(10) . . . . ?
C7 C8 C9 C10 0.24(17) . . . . ?
C7 C12 C13 C14 67.38(12) . . . . ?
C7 C12 C15 C16 62.67(13) . . . . ?
C8 C7 C12 C13 -82.88(12) . . . . ?
C8 C7 C12 C15 42.83(13) . . . . ?
C8 C9 C10 C11 1.09(17) . . . . ?
C9 C10 C11 C6 -0.62(17) . . . . ?
C9 C10 C11 C17 -178.54(10) . . . . ?
C10 C11 C17 C18 88.18(12) . . . . ?
C10 C11 C17 C20 -38.64(15) . . . . ?
C11 C6 C7 C8 2.42(15) . . . . ?
C11 C6 C7 C12 -174.83(9) . . . . ?
C11 C17 C18 C19 -66.84(13) . . . . ?
C11 C17 C20 C21 -62.30(14) . . . . ?
C12 C7 C8 C9 175.32(10) . . . . ?
C13 C12 C15 C16 -171.67(10) . . . . ?
C15 C12 C13 C14 -60.62(12) . . . . ?
C18 C17 C20 C21 171.25(11) . . . . ?
C20 C17 C18 C19 61.55(13) . . . . ?
C22 N2 C4 C3 -165.28(10) . . . . ?
C22 N2 C4 C5 16.22(14) . . . . ?
C22 C23 C24 C25 0.47(16) . . . . ?
C22 C23 C28 C29 -115.64(11) . . . . ?
C22 C23 C28 C31 121.16(11) . . . . ?
C22 C27 C33 C34 139.91(10) . . . . ?
C22 C27 C33 C36 -95.99(11) . . . . ?
C23 C22 C27 C26 3.49(15) . . . . ?
C23 C22 C27 C33 -179.95(9) . . . . ?
C23 C24 C25 C26 1.93(17) . . . . ?
C23 C28 C29 C30 59.74(12) . . . . ?
C23 C28 C31 C32 -176.18(10) . . . . ?
C24 C23 C28 C29 64.69(12) . . . . ?
C24 C23 C28 C31 -58.52(13) . . . . ?
C24 C25 C26 C27 -1.62(17) . . . . ?
C25 C26 C27 C22 -1.07(16) . . . . ?
C25 C26 C27 C33 -177.69(10) . . . . ?
C26 C27 C33 C34 -43.56(13) . . . . ?
C26 C27 C33 C36 80.53(12) . . . . ?
C27 C22 C23 C24 -3.19(15) . . . . ?
C27 C22 C23 C28 177.13(9) . . . . ?
C27 C33 C34 C35 -57.49(13) . . . . ?
C27 C33 C36 C37 166.35(10) . . . . ?
C28 C23 C24 C25 -179.84(10) . . . . ?
C29 C28 C31 C32 61.02(13) . . . . ?
C31 C28 C29 C30 -177.20(10) . . . . ?
C34 C33 C36 C37 -68.16(13) . . . . ?
C36 C33 C34 C35 178.96(10) . . . . ?
C38 O2 C42 C41 -57.80(12) . . . . ?
C38 C39 C40 C41 53.24(13) . . . . ?
C39 C40 C41 C42 -52.02(13) . . . . ?
C40 C41 C42 O2 54.52(13) . . . . ?
C42 O2 C38 C39 59.62(12) . . . . ?
C43 C44 C45 C45 175.10(16) . . . 2_675 ?
C43 C44A C45A C45A -174(2) . . . 2_675 ?

_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 0.000 228.5 50.9 '1 hexane'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-10-28
_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 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_chemical_properties_physical    Moisture-sensitive
