Open metal sites dangled on cobalt trigonal prismatic clusters within porous MOF for CO2 capture
Gao, Wen-Yang; Palakurty, Sathvik; Wojtas, Lukasz; Chen, Yu-Sheng; Ma, Shengqian; Inorganic Chemistry Frontiers 2 (2015) 369–; doi:10.1039/C4QI00240G

data_4348420
_publ_section_title
;
 Open metal sites dangled on cobalt trigonal prismatic clusters within
 porous MOF for CO2 capture
;
_journal_issue                   4
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              369
_journal_paper_doi               10.1039/C4QI00240G
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety
'0.25(C211.01 H72 Co16 N6.34 O86.77), 1.07(C3 N O), 1.92(O), 0.2(C)'
_chemical_formula_sum            'C56.15 H18 Co4 N2.65 O24.68'
_chemical_formula_weight         1360.22
_chemical_melting_point          Not
_chemical_name_common            Co_Pyrene_1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-31 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.152(2)
_cell_length_b                   14.4302(10)
_cell_length_c                   14.0799(10)
_cell_measurement_temperature    100(2)
_cell_volume                     6735.7(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1844
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            108920
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        14.240
_diffrn_reflns_theta_max         14.241
_diffrn_reflns_theta_min         1.362
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.241
_exptl_crystal_colour            Light
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6143
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+30.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4535
_reflns_number_total             6143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4qi00240g2.cif
_cod_data_source_block           co_wy17_2
_cod_original_cell_volume        6735.6(8)
_cod_database_code               4348420
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.994
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N9-C1C
 1.32 with sigma of 0.02
 N9-C2 = N9-C1
 1.45 with sigma of 0.02
 O12-C1C
 1.23 with sigma of 0.02
 O43A-C45A
 1.4 with sigma of 0.02
 N2-C1A
 1.5 with sigma of 0.02
 N2-C1B
 1.32 with sigma of 0.02
 O11-C1B
 1.23 with sigma of 0.02
 C19-N2
 1.45 with sigma of 0.02
 N2-C1A
 1.45 with sigma of 0.02
 N14-C4 = N14-C5
 1.45 with sigma of 0.02
 N3-C1D = N3-C35
 1.45 with sigma of 0.02
 O3B-C1G
 1.23 with sigma of 0.02
 N3-C1G
 1.32 with sigma of 0.02
 N15-C42 = N15-C43
 1.5 with sigma of 0.02
 O32-C1E
 1.23 with sigma of 0.02
 N14-C1E
 1.32 with sigma of 0.02
 C4-C5
 2.47 with sigma of 0.04
 N14-O32
 2.26 with sigma of 0.04
 C35-C1D
 2.47 with sigma of 0.04
 N3-O3B
 2.26 with sigma of 0.04
 C35-C1G
 2.41 with sigma of 0.04
 C1G-C1D
 2.41 with sigma of 0.04
 C1E-C4
 2.41 with sigma of 0.04
 C5-C1E
 2.41 with sigma of 0.04
3. Restrained planarity
 O3B, C1G, N3, C35, C1D
 with sigma of 0.04
 O32, C1E, N14, C4, C5
 with sigma of 0.04
4. Rigid bond restraints
 C3, N6, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C5 \\sim N14: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1G \\sim N3 \\sim C1D \\sim C35 \\sim O3B: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O10 \\sim O43A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O1G \\sim O1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O45) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.005
6. Others
 1*[Sof(Co4)]+1*[Sof(Co6)]+1*[Sof(Co5)]=1 with esd of 0
 Sof(O44)=Sof(C43)=Sof(C44)=Sof(C42)=Sof(N15)=0.5*FVAR(5)
 Fixed Sof: O1B(0.1515) O11(0.16667) C39(0.2) O10(0.2) C3(0.2) C40(0.2)
 N6(0.2) N14(0.25) O14(0.125) C2(0.33333) O2(0.16666) C1(0.33333) N9(0.33333)
 O12(0.16666) C19(0.16667) N2(0.16667) C1A(0.16667) C1B(0.16667) C1E(0.25)
 C1G(0.25) C1C(0.33333) N3(0.25) C1D(0.25) C35(0.25) O18(0.25) C4(0.25)
 C5(0.25) O16(0.0625) O1D(0.125) O1E(0.125) O1G(0.1515) C45A(0.1) O46(0.1)
7.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C16(H16), C23(H23), C25(H25), C28(H28), C29(H29),
 C33(H33), C38(H38)
;
_olex2_submission_special_instructions 'No special instructions were received'