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_4510165
_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         'C24 H28 B18 Co O8, 3(C24 H20 P)'
_chemical_formula_sum            'C96 H88 B18 Co O8 P3'
_chemical_formula_weight         1716.08
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-15
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                79.3640(10)
_cell_angle_beta                 73.3530(10)
_cell_angle_gamma                73.1420(10)
_cell_formula_units_Z            4
_cell_length_a                   22.3221(4)
_cell_length_b                   22.7490(4)
_cell_length_c                   22.8496(4)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.68
_cell_measurement_theta_min      2.56
_cell_volume                     10573.7(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
;
XL, 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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65069
_diffrn_reflns_theta_full        62.38
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         2.03
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.7967.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2574
_refine_ls_number_reflns         32184
_refine_ls_number_restraints     1354
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2469
_reflns_number_gt                20134
_reflns_number_total             32184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            PPh4[5].cif
_cod_data_source_block           n1843a
_cod_database_code               4510165
_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 = 2368.9 Ang^3^ [22.4%]
Total electron count / cell = 392.7
;