Metallacarborane-Based Metal‒Organic Framework with a Complex Topology
Kennedy, Robert D.; Clingerman, Daniel J.; Morris, William; Wilmer, Christopher E.; Sarjeant, Amy A.; Stern, Charlotte L.; O’Keeffe, Michael; Snurr, Randall Q.; Hupp, Joseph T.; Farha, Omar K.; Mirkin, Chad A.; Crystal Growth & Design 14 (2014) 1324–; doi:10.1021/cg401817g

data_4510166
_publ_section_title
;
 Metallacarborane-Based Metal--Organic Framework with a Complex Topology
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1324
_journal_paper_doi               10.1021/cg401817g
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C72 H78 B54 Co3 Cu6 O30'
_chemical_formula_sum            'C72 H78 B54 Co3 Cu6 O30'
_chemical_formula_weight         2565.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.549(3)
_cell_length_b                   38.148(3)
_cell_length_c                   55.536(4)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.49
_cell_measurement_theta_min      2.80
_cell_volume                     77432(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.339
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1579
_diffrn_reflns_av_unetI/netI     0.1421
_diffrn_reflns_Laue_measured_fraction_full 0.339
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            63589
_diffrn_reflns_point_group_measured_fraction_full 0.339
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         39.97
_diffrn_reflns_theta_min         1.40
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1648 before and 0.1033 after correction.
The Ratio of minimum to maximum transmission is 0.5833.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.440
_exptl_crystal_description       block
_exptl_crystal_F_000             10200
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         12416
_refine_ls_number_restraints     3702
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0939
_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^)+(0.1571P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6289
_reflns_number_total             12416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NU-152.cif
_cod_data_source_block           n2002a_a
_cod_original_cell_volume        77431(10)
_cod_database_code               4510166
_refinement_special_details
;
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Restrained distances
 B26-B27 \\sim B22-B27 \\sim B26-B22 \\sim B25-B23 \\sim B25-B26 \\sim B23-B22 
 \\sim B23-B24 \\sim B25-B24
 \\sim B20-B24 \\sim B19-B24 \\sim B19-B23 \\sim B19-B20 \\sim B19-B21 
 \\sim B20-B21 \\sim B21-B27 \\sim B22-
 B21 \\sim B19-B22 \\sim B4-B1 \\sim B5-B1 \\sim B6-B1 \\sim B2-B6 \\sim B2-B1 
 \\sim B3-B1 \\sim B2-B3 \\sim B3-B4
 \\sim B4-B9 \\sim B5-B4 \\sim B5-B8 \\sim B5-B9 \\sim B5-B6 \\sim B6-B8 
 \\sim B8-B9 \\sim B6-B7 \\sim B7-B8 \\sim B2-
 B7 \\sim B16-B10 \\sim B15-B10 \\sim B15-B11 \\sim B16-B15 \\sim B14-B15 
 \\sim B14-B11 \\sim B12-B11 \\sim B14-
 B12 \\sim B14-B13 \\sim B12-B13 \\sim B13-B18 \\sim B17-B18 \\sim B17-B13 
 \\sim B11-B10 \\sim B17-B16 -
 B16-B18 \\sim B14-B18 \\sim B15-B18 \\sim B21A-B19A \\sim B20A-B19A \\sim 
 B21A-B20A \\sim B22A-B21A -
 B22A-B19A \\sim B23A-B22A \\sim B23A-B19A \\sim B24A-B19A \\sim B24A-B23A 
 \\sim B24A-B20A \\sim B25A-
 B24A \\sim B25A-B23A \\sim B26A-B23A \\sim B26A-B22A \\sim B27A-B22A \\sim 
 B27A-B21A \\sim B27A-B26A -
 B26A-B25A
 with sigma of 0.02
 C13-B9 \\sim C13-B4 \\sim C13-B3 \\sim C12-B3 \\sim C12-B2 \\sim C12-B7 \\sim 
 C14-B10 \\sim C14-B16 \\sim C14-
 B17 \\sim C15-B17 \\sim C15-B13 \\sim C15-B12 \\sim C35-B20 \\sim C35-B21 
 \\sim C34-B20 \\sim C34-B24 -
 C34-B25 \\sim C35-B27 \\sim C34A-B24A \\sim C34A-B25A \\sim C35A-B21A \\sim 
 C35A-B20A \\sim C34A-B20A
 \\sim C35A-B27A
 with sigma of 0.02
 C12-C13 \\sim C14-C15 \\sim C35-C34 \\sim C35A-C34A
 with sigma of 0.02
 Co2-C35 \\sim Co2-C34 \\sim Co1-C13 \\sim Co1-C12 \\sim Co1-C14 \\sim Co1-C15 
 \\sim Co2-C34A \\sim Co2-C35A
 with sigma of 0.02
 Co1-B9 \\sim Co1-B8 \\sim Co1-B7 \\sim Co1-B12 \\sim Co1-B11 \\sim Co1-B10 
 \\sim Co2-B27 \\sim Co2-B26 -
 Co2-B25 \\sim Co2-B25A \\sim Co2-B26A \\sim Co2-B27A
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and 
sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: C34(0.5) H34(0.5) C34A(0.5) H34A(0.5) C35(0.5) H35(0.5) C35A(0.5)
 H35A(0.5) B19(0.5) B19A(0.5) B20(0.5) H20(0.5) B20A(0.5) H20A(0.5) B21(0.5)
 H21A(0.5) B21A(0.5) H21B(0.5) B22(0.5) H22(0.5) B22A(0.5) H22A(0.5) B23(0.5)
 H23A(0.5) B23A(0.5) H23B(0.5) B24(0.5) H24(0.5) B24A(0.5) H24A(0.5) B25(0.5)
 H25(0.5) B25A(0.5) H25A(0.5) B26(0.5) H26A(0.5) B26A(0.5) H26B(0.5) B27(0.5)
 H27(0.5) B27A(0.5) H27A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C19(H19), C21(H21), C23(H23), C26(H26), C28(H28),
 C30(H30)
6.b Boron cage BH refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C34(H34), C34A(H34A), C35(H35),
 C35A(H35A), B2(H2), B3(H3), B4(H4A), B5(H5), B6(H6A), B7(H7), B8(H8A), B9(H9),
 B10(H10), B11(H11), B12(H12A), B13(H13A), B14(H14A), B15(H15A), B16(H16),
 B17(H17), B20(H20), B20A(H20A), B21(H21A), B21A(H21B), B22(H22), B22A(H22A),
 B23(H23A), B23A(H23B), B24(H24), B24A(H24A), B25(H25), B25A(H25A), B26(H26A),
 B26A(H26B), B27(H27), B27A(H27A)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 60520.3 Ang^3^ [78.2%]
Total electron count / cell = 19471.7
;
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.408
_shelxl_version_number           2012-9