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_7702236
_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 Mn5 N12 O12, 4(Cl1 O4), 10 C H4 O'
_chemical_formula_sum            'C82 H112 Cl4 Cr2 Mn5 N12 O38'
_chemical_formula_weight         2394.33
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_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
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.7045(6)
_cell_length_b                   14.7045(6)
_cell_length_c                   38.106(5)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      50.1250
_cell_measurement_theta_min      4.1470
_cell_volume                     7135.5(10)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.3322
_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    -96.00  -2.00   1.00   10.00    --  -43.17 125.00  30.00   94
  2  \w   -130.00  43.00   1.00   10.00    --  -43.17   0.00  60.00  173
  3  \w    -66.00  29.00   1.00   10.00    --  -43.17  38.00 -60.00   95
  4  \w     23.00  98.00   1.00   10.00    --   43.17-125.00-120.00   75
  5  \w     23.00  98.00   1.00   10.00    --   43.17-125.00  60.00   75
  6  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00 -30.00   95
  7  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00  90.00   98
  8  \w     37.00 142.00   1.00   30.00    --  111.00 -77.00-150.00  105
  9  \w     36.00 135.00   1.00   30.00    --  111.00 -30.00-150.00   99
 10  \w     87.00 178.00   1.00   30.00    --  111.00  30.00 -90.00   91
 11  \w     80.00 178.00   1.00   30.00    --  111.00  77.00-150.00   98
 12  \w     94.00 178.00   1.00   30.00    --  111.00 125.00 -90.00   84
 13  \w     39.00 121.00   1.00   30.00    --  111.00-125.00  30.00   82
 14  \w     87.00 178.00   1.00   30.00    --  111.00  30.00-180.00   91
 15  \w     39.00 121.00   1.00   30.00    --  111.00-125.00-150.00   82
 16  \w     94.00 178.00   1.00   30.00    --  111.00 125.00 150.00   84
 17  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00  60.00   79
 18  \w   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00-120.00   96
 19  \w   -117.00 -12.00   1.00   10.00    --  -43.17 -77.00  90.00  105
 20  \w   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00 -30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0145418000
_diffrn_orient_matrix_UB_12      0.0417511000
_diffrn_orient_matrix_UB_13      -0.0379047000
_diffrn_orient_matrix_UB_21      -0.1192148000
_diffrn_orient_matrix_UB_22      -0.0439265000
_diffrn_orient_matrix_UB_23      -0.0030012000
_diffrn_orient_matrix_UB_31      0.0139978000
_diffrn_orient_matrix_UB_32      0.1045978000
_diffrn_orient_matrix_UB_33      0.0138866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        50.499
_diffrn_reflns_theta_max         50.499
_diffrn_reflns_theta_min         3.479
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.898
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_correction_T_min  0.2634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0991 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.3016.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       plate
_exptl_crystal_F_000             3699
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.024
_platon_squeeze_details          '10 MeOH per wheel'
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0737
_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/[\s^2^(Fo^2^)+(0.1734P)^2^+32.5148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1482
_reflns_number_total             1673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           3
_cod_original_cell_volume        7135.4(11)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702236
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H30 N10 O10 Mn Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 749o'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.712(4)
 0.288(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Shared sites
{Mn1, Cr1}
4. Uiso/Uaniso restraints and constraints
Uanis(Mn1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, Cl2, Cl2, O5, O5, O6, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl1, Cl1, O4, O4, O3, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, N2A, C7A, C12A, C11A, C8A, C10A, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, N2, C7, C12, C11, C8, C10, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O2, N2, C7, C12, C11, C8, C10, C9} sigma for 1-2: 0.02, 1-3: 0.02
as
{O2A, N2A, C7A, C12A, C11A, C8A, C10A, C9A}
7. Others
 Sof(O2A)=Sof(N2A)=Sof(C7A)=Sof(H7A)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C11A)=
 Sof(C8A)=Sof(H8A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=1-FVAR(1)
 Sof(O2)=Sof(N2)=Sof(C7)=Sof(H7)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(C8)=
 Sof(H8)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=FVAR(1)
 Fixed Sof: Mn1(0.66666) Cr1(0.33333)
8.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12A(H12C,H12D), C6(H6A,H6B)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C9(H9), C7A(H7A), C8A(H8A), C10A(H10A), C9A(H9A),
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              54124
_shelx_fab_checksum              97632
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2016-10-05
_olex2_date_sample_submission    2016-10-05
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 749o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.330
_oxdiff_exptl_absorpt_empirical_full_min 0.624