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_4510167
_publ_section_title
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 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         'C24 H26 B18 Co Cu2 O10'
_chemical_formula_sum            'C24 H26 B18 Co Cu2 O10'
_chemical_formula_weight         855.04
_chemical_name_systematic
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 ?
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_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2013-06-14
_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                120
_cell_formula_units_Z            6
_cell_length_a                   18.248(2)
_cell_length_b                   18.248(2)
_cell_length_c                   47.113(7)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.92
_cell_measurement_theta_min      2.80
_cell_volume                     13586(3)
_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
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0791
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            29065
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        40.120
_diffrn_reflns_theta_max         40.12
_diffrn_reflns_theta_min         0.94
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.133
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.6354.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.627
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2550
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00016(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.778
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     1740
_refine_ls_restrained_S_all      2.247
_refine_ls_R_factor_all          0.2107
_refine_ls_R_factor_gt           0.1544
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.4582
_refine_ls_wR_factor_ref         0.4944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1322
_reflns_number_total             2782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NU-151.cif
_cod_data_source_block           n2002
_cod_original_cell_volume        13586(4)
_cod_database_code               4510167
_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
 C12A-C12A_$1 = C12A-B7A_$1 = C11A-B7A_$1 = C11A-B8A_$1 = B9A-B8A_$1 = B9A-
 B9A_$1 = B8A-B9A_$1 = B8A-C11A_$1 = B7A-C11A_$1 = B7A-C12A_$1
 3.15 with sigma of 0.0001
 B5A-B1A \\sim B4A-B1A \\sim B3A-B1A \\sim B9A-B3A \\sim B6A-B1A \\sim B6A-B5A 
 \\sim B4A-B3A \\sim B5A-B4A
 \\sim B2A-B1A \\sim B3A-B2A \\sim B6A-B2A \\sim B7A-B6A \\sim B7A-B2A
 \\sim B8A-B2A \\sim B8A-B3A \\sim B9A-
 B4A \\sim B9A-B8A \\sim B8A-B7A \\sim B5-B1 \\sim B6-B1 \\sim B2-B1 
 \\sim B3-B2 \\sim B4-B1 \\sim B5-B4 \\sim B6-
 B5 \\sim B6-B2 \\sim B7-B2 \\sim B8-B2 \\sim B8-B3 \\sim B9-B3 \\sim B9-B4
 \\sim B7-B6 \\sim B9-B8 \\sim B8-B7 -
 B3-B1 \\sim B4-B3
 with sigma of 0.02
 C11-B9 \\sim C11-B4 \\sim C11-B5 \\sim C12-B5 \\sim C12-B6 \\sim C12-B7 
 \\sim C11A-B9A \\sim C11A-B4A -
 C11A-B5A \\sim C12A-B5A \\sim C12A-B6A \\sim C12A-B7A
 with sigma of 0.02
 Co1A-B7A \\sim Co1A-B8A \\sim Co1A-B9A \\sim Co1-B9 \\sim Co1-B8 \\sim Co1-B7
 with sigma of 0.02
 Co1-C11 \\sim Co1-C12 \\sim Co1A-C11A \\sim Co1A-C12A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C10A-B1A \\sim C10-B1
 with sigma of 0.02
 C9-C10A \\sim C9-C10
 with sigma of 0.02
 C3-C2 \\sim C7-C2 \\sim C7-C6 \\sim C6-C5 \\sim C5-C4 \\sim C4-C3
 with sigma of 0.02
 C2-C6 \\sim C7-C5 \\sim C6-C4 \\sim C5-C3 \\sim C4-C2 \\sim C3-C7
 with sigma of 0.02
 O1-C1 \\sim O2-C1 \\sim O3-C8 \\sim O4-C8
 with sigma of 0.02
 C8-C4 \\sim C2-C1
 with sigma of 0.02
 C10-B2 \\sim C10-B3 \\sim C10-B4 \\sim C10-B5 \\sim C10-B6 \\sim C10A-B2A 
 \\sim C10A-B3A \\sim C10A-B4A -
 C10A-B5A \\sim C10A-B6A
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C7, C6, C8
 with sigma of 0.1
 B1A, C10A, C9, C6, C7, C2, C3, C4, C5, C8, O4, O3, C1, O1, O2
 with sigma of 0.1
 B1, C10, C9, C6, C5, C4, C3, C2, C7, C8, O4, O3, C1, O1, O2
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and 
sigma for terminal atoms of 0.08
6. Others
 Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(B1A)=Sof(B2A)=Sof(H2A)=
 Sof(B3A)=Sof(H3AA)=Sof(B4A)=Sof(H4A)=Sof(B5A)=Sof(H5AA)=Sof(B6A)=Sof(H6A)=
 Sof(B7A)=Sof(H7AA)=Sof(B8A)=Sof(H8A)=Sof(B9A)=Sof(H9A)=1-FVAR(1)
 Sof(Co1A)=0.5*(1-FVAR(2))
 Sof(Co1)=0.5*FVAR(2)
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(B1)=Sof(B2)=Sof(H2)=Sof(B3)=
 Sof(H3A)=Sof(B4)=Sof(H4)=Sof(B5)=Sof(H5A)=Sof(B6)=Sof(H6)=Sof(B7)=Sof(H7A)=
 Sof(B8)=Sof(H8)=Sof(B9)=Sof(H9)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
7.b Boron cage BH refined with riding coordinates:
 C11(H11), C12(H12), C11A(H11A), C12A(H12A), B2(H2), B3(H3A), B4(H4), B5(H5A),
 B6(H6), B7(H7A), B8(H8), B9(H9), B2A(H2A), B3A(H3AA), B4A(H4A), B5A(H5AA),
 B6A(H6A), B7A(H7AA), B8A(H8A), B9A(H9A)
;
_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.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 8835.7 Ang^3^ [65.0%]
Total electron count / cell = 1602.3
;
_shelxl_version_number           2012-9