A Mixed-Cluster Approach for Building a Highly Porous Cobalt(II) Isonicotinic Acid Framework: Gas Sorption Properties and Computational Analyses
Chen, Di-Ming; Zhang, Nan-Nan; Liu, Chun-Sen; Jiang, Zhi-Hao; Wang, Xing-Dong; Du, Miao; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b03170

data_4345241
_publ_section_title
;
 A Mixed-Cluster Approach for Building a Highly Porous Cobalt(II)
 Isonicotinic Acid Framework: Gas Sorption Properties and Computational
 Analyses
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b03170
_journal_year                    2017
_chemical_formula_moiety         '0.5(C96 H64 Co16 N16 O50)'
_chemical_formula_sum            'C48 H32 Co8 N8 O25'
_chemical_formula_weight         1592.25
_space_group_crystal_system      tetragonal
_space_group_IT_number           119
_space_group_name_Hall           'I -4 -2'
_space_group_name_H-M_alt        'I -4 m 2'
_symmetry_space_group_name_Hall  'I -4 -2'
_symmetry_space_group_name_H-M   'I -4 m 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3699(10)
_cell_length_b                   17.3699(10)
_cell_length_c                   19.8944(12)
_cell_measurement_reflns_used    2228
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7730
_cell_measurement_theta_min      3.6980
_cell_volume                     6002.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3031
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -17.00   10.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7729  -99.0000 -150.0000 27

  2 omega  -61.00   32.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7729  -57.0000   30.0000 93

  3 omega  -28.00    3.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7729   19.0000  -90.0000 31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0371904000
_diffrn_orient_matrix_UB_12      -0.0119397000
_diffrn_orient_matrix_UB_13      0.0104166000
_diffrn_orient_matrix_UB_21      0.0098991000
_diffrn_orient_matrix_UB_22      0.0078495000
_diffrn_orient_matrix_UB_23      0.0338974000
_diffrn_orient_matrix_UB_31      -0.0136381000
_diffrn_orient_matrix_UB_32      0.0382546000
_diffrn_orient_matrix_UB_33      -0.0037129000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9679
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         3.665
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.881
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1584
_platon_squeeze_details
;
;
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1085P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2135
_reflns_number_total             2825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03170_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        6002.4(8)
_cod_database_code               4345241
_chemical_oxdiff_formula         'C H O N Co'
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C00H \\sim C9 \\sim C14 \\sim C00G \\sim N008 \\sim C00B: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C00A \\sim C00F \\sim C00E: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O00) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(C00G)=Sof(H00G)=Sof(C00H)=Sof(H00H)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C14)=Sof(H14)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C9(H9), C14(H14)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'