Cages on a plane: a structural matrix for molecular 'sheets'.
Fraser, Hector W. L.; Nichol, Gary S.; Baldansuren, Amgalanbaatar; McInnes, Eric J. L.; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15530–15537; doi:10.1039/c8dt03793k

data_7702237
_publ_section_title
;
 Cages on a plane: a structural matrix for molecular 'sheets'.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15530
_journal_page_last               15537
_journal_paper_doi               10.1039/c8dt03793k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C72 H72 Cr2 Cu5 N12 O12, 2(Cl O4), 2(N O3)'
_chemical_formula_sum            'C72 H72 Cl2 Cr2 Cu5 N14 O26'
_chemical_formula_weight         2042.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.268(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5052(12)
_cell_length_b                   25.0735(19)
_cell_length_c                   25.095(5)
_cell_measurement_reflns_used    2785
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7110
_cell_measurement_theta_min      4.9380
_cell_volume                     9127(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -75.00  31.00   1.00   10.00    --  -43.17  77.00 -30.00  106
  2  \w    -70.00  27.00   1.00   10.00    --  -43.17  57.00  90.00   97
  3  \w   -117.00 -12.00   1.00   10.00    --  -43.17 -77.00  30.00  105
  4  \w     83.00 178.00   1.00   30.00    --  111.00  61.00 -90.00   95
  5  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00-150.00   79
  6  \w     94.00 178.00   1.00   30.00    --  111.00 125.00  60.00   84
  7  \w     87.00 178.00   1.00   30.00    --  111.00  45.00 -30.00   91
  8  \w   -113.00 -56.00   1.00   10.00    --  -43.17 -57.00-150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007490000
_diffrn_orient_matrix_UB_12      0.0065664000
_diffrn_orient_matrix_UB_13      -0.0610059000
_diffrn_orient_matrix_UB_21      0.1060858000
_diffrn_orient_matrix_UB_22      0.0025256000
_diffrn_orient_matrix_UB_23      0.0011509000
_diffrn_orient_matrix_UB_31      0.0046520000
_diffrn_orient_matrix_UB_32      -0.0610871000
_diffrn_orient_matrix_UB_33      -0.0064155000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18466
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.751
_diffrn_reflns_theta_min         3.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plate
_exptl_crystal_F_000             4148
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.026
_refine_diff_density_max         4.515
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         18466
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.451
_refine_ls_R_factor_all          0.3043
_refine_ls_R_factor_gt           0.2142
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5029
_refine_ls_wR_factor_ref         0.5502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6177
_reflns_number_total             18466
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 120.0851\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
Component 3 rotated by -119.9041\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.01 -0.00 1.00] (direct)
;
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           4
_cod_database_code               7702237
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cu Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 719o'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(5)
 0.126(3) 0.311(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C12-C11 = C6-C5 = C18-C17 = C36-C35 = C30-C29 = C24-C23
 1.51 with sigma of 0.02
 O1-C6 = O2-C12 = O6-C36 = O5-C30 = O3-C18 = O4-C24
 1.41 with sigma of 0.02
 Cl1-O9 = Cl1-O8 = Cl1-O10 = Cl1-O7
 1.41 with sigma of 0.02
 O11-N7 = O12-N7 = O13-N8 = O14-N8
 1.24 with sigma of 0.02
 O9-O8 = O10-O7
 2.28 with sigma of 0.04
 O9-O10 = O8-O7
 2.28 with sigma of 0.04
 O10-O8 = O9-O7
 2.28 with sigma of 0.04
 O14-O13 = O12-O11
 2.14 with sigma of 0.04
4. Others
 Fixed Uiso: C34(0.23954)
5.a Everything fixed:
 N8, O14, O13, N7, O12, O11
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C9(H9), C8(H8), C7(H7), C13(H13),
 C14(H14), C15(H15), C16(H16), C22(H22), C21(H21), C20(H20), C19(H19), C28(H28),
  C27(H27), C26(H26), C25(H25), C34(H34), C33(H33), C32(H32), C31(H31)
5.d Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C11,C10,C9,C8,C7), N3(C13,C14,C15,C16,C17), N4(C23,C22,
 C21,C20,C19), N5(C29,C28,C27,C26,C25), N6(C35,C34,C33,C32,C31)
;
_shelx_res_checksum              47598
_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 1.682
_oxdiff_exptl_absorpt_empirical_full_min 0.384
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3