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_7702240
_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 Al2 Co5 N12 O12, 4(Cl1 O4), 9 (C H4 O)'
_chemical_formula_sum            'C81 H108 Al2 Cl4 Co5 N12 O37'
_chemical_formula_weight         2332.20
_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     dual
_audit_creation_date             2016-11-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_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                   14.6812(5)
_cell_length_b                   14.6812(5)
_cell_length_c                   38.0235(14)
_cell_measurement_reflns_used    12096
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      26.1220
_cell_measurement_theta_min      3.1830
_cell_volume                     7097.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  30.00   1.00   30.00    --   -9.43 -99.00  90.00   50
  2  \w    -80.00   5.00   1.00   30.00    --   -9.43 -57.00 150.00   85
  3  \w    -34.00  -5.00   1.00   30.00    --   -9.43  48.00 -80.39   29
  4  \w     21.00  48.00   1.00   30.00    --   10.84-140.00-170.98   27
  5  \w    -40.00 -13.00   1.00   30.00    --   10.84 -77.00 -90.00   27
  6  \w      0.00  27.00   1.00   30.00    --   10.84 -88.00 170.93   27
  7  \w    -40.00  42.00   1.00   30.00    --   10.84 -77.00-150.00   82
  8  \w     43.00  82.00   1.00   30.00    --   10.84  38.00-120.00   39
  9  \w    -45.00 -18.00   1.00   30.00    --   10.84 -38.00-150.00   27
 10  \w     24.00  51.00   1.00   30.00    --   10.84  38.00-150.00   27
 11  \w      2.00  65.00   1.00   30.00    --   10.84-124.00 102.42   63
 12  \w    -62.00  32.00   1.00   30.00    --   10.84 -38.00 -60.00   94
 13  \w    -37.00 -10.00   1.00   30.00    --   10.84 -77.00 120.00   27
 14  \w     38.00  65.00   1.00   30.00    --   10.84  19.00 -30.00   27
 15  \w     46.00  80.00   1.00   30.00    --   10.84  19.00 -60.00   34
;
_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      -0.0220616000
_diffrn_orient_matrix_UB_12      -0.0287998000
_diffrn_orient_matrix_UB_13      0.0156924000
_diffrn_orient_matrix_UB_21      0.0334685000
_diffrn_orient_matrix_UB_22      -0.0218039000
_diffrn_orient_matrix_UB_23      -0.0012383000
_diffrn_orient_matrix_UB_31      0.0387856000
_diffrn_orient_matrix_UB_32      0.0425051000
_diffrn_orient_matrix_UB_33      0.0100107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            38106
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.340
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         3.121
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       plate
_exptl_crystal_F_000             3609
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0429P)^2^+68.7616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2560
_reflns_number_total             2893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03793k2.cif
_cod_data_source_block           5
_cod_original_cell_volume        7097.5(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702240
_chemical_oxdiff_formula         'C60 H100 N10 O30 Co6 Cl Al2'
_chemical_oxdiff_usercomment     '@ 120 K 756o'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Co1, Al1}
3. Restrained distances
 Cl2-O5A \\sim Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Al1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O5A, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O5A)=1-FVAR(1)
 Sof(O5)=FVAR(1)
 Fixed Sof: Co1(0.66666) Al1(0.33333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              68836
_shelx_fab_checksum              62147
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-17
_olex2_date_sample_submission    2016-10-14
_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 '756o SOB'
_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.737