Exchange coupled Co(ii) based layered and porous metal-organic frameworks: structural diversity, gas adsorption, and magnetic properties.
Kharwar, Ajit Kumar; Konar, Sanjit; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4012–4021; doi:10.1039/d0dt00211a

data_7703626
_publ_section_title
;
 Exchange coupled Co(ii) based layered and porous metal-organic
 frameworks: structural diversity, gas adsorption, and magnetic
 properties.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4012
_journal_page_last               4021
_journal_paper_doi               10.1039/d0dt00211a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H43 Co2 N3 O9, 4[CH3CN]'
_chemical_formula_sum            'C50 H55 Co2 N7 O9'
_chemical_formula_weight         1015.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-01
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-02 deposited with the CCDC.	2020-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                85.585(5)
_cell_angle_beta                 65.242(3)
_cell_angle_gamma                88.095(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6375(16)
_cell_length_b                   13.5987(17)
_cell_length_c                   15.052(3)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.26
_cell_volume                     2342.0(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_unetI/netI     0.1212
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30870
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         2.191
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.51
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         7659
_refine_ls_number_restraints     730
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.1141
_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^)+(0.0949P)^2^+28.4486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_ref         0.2759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4930
_reflns_number_total             7659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00211a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7703626--7703629.cif.'
_cod_original_cell_volume        2342.1(6)
_cod_database_code               7703626
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C3, C21B}
{C6, C23B}
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C21B)
Uanis(C6) = Uanis(C23B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: C3(0.6) C13A(0.7) C6(0.6) C11A(0.7) C12A(0.7) C19(0.6) H19(0.6)
 C20(0.6) H20(0.6) C122(0.7) H12A(0.7) H12B(0.7) H12C(0.7) C23(0.6) H23(0.6)
 C22(0.6) H22(0.6) C14A(0.7) H14A(0.7) H14B(0.7) C4(0.6) H4A(0.6) H4B(0.6)
 C5(0.6) H5A(0.6) H5B(0.6) C15A(0.7) H15A(0.7) H15B(0.7) C121(0.7) H12D(0.7)
 H12E(0.7) H12F(0.7) C7(0.6) C16(0.4) H16A(0.4) H16B(0.4) H16C(0.4) C17(0.6)
 H17A(0.6) H17B(0.6) H17C(0.6) C1B(0.3) C3B(0.3) C2B(0.3) C8(0.3) H8A(0.3)
 H8B(0.3) H8C(0.3) C5B(0.3) H5BA(0.3) H5BB(0.3) C4B(0.3) H4BA(0.3) H4BB(0.3)
 C13(0.3) H13A(0.3) H13B(0.3) H13C(0.3) C1A3(0.35) H1AA(0.35) H1AB(0.35)
 H1AC(0.35) C1A1(0.35) H1AD(0.35) H1AE(0.35) H1AF(0.35) C21B(0.4) C23B(0.4)
 C25B(0.4) H25A(0.4) H25B(0.4) C24B(0.4) H24A(0.4) H24B(0.4) C22B(0.4)
 C16A(0.4) H16D(0.4) H16E(0.4) H16F(0.4) C17A(0.6) H17D(0.6) H17E(0.6)
 H17F(0.6) C20A(0.4) H20A(0.4) C23A(0.4) H23A(0.4) C22A(0.4) H22A(0.4)
 C19A(0.4) H19A(0.4) C41(0.3) H41A(0.3) H41B(0.3) H41C(0.3) C44(0.3) H44A(0.3)
 H44B(0.3) H44C(0.3) C46(0.2) H46A(0.2) H46B(0.2) H46C(0.2) C45(0.2) H45A(0.2)
 H45B(0.2) H45C(0.2) C13B(0.15) H13D(0.15) H13E(0.15) H13F(0.15) C11B(0.15)
 H11A(0.15) H11B(0.15) H11C(0.15)
6.a Riding coordinates:
 C1A3(H1AA,H1AB,H1AC), C13B(H13D,H13E,H13F), C11B(H11A,H11B,H11C)
6.b Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C4(H4A,H4B), C5(H5A,H5B), C15A(H15A,H15B), C5B(H5BA,H5BB),
 C4B(H4BA,H4BB), C25B(H25A,H25B), C24B(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C27(H27), C31(H31), C30(H30), C32(H32), C39(H39), C33(H33),
 C19(H19), C20(H20), C35(H35), C23(H23), C36(H36), C22(H22), C38(H38),
 C20A(H20A), C23A(H23A), C22A(H22A), C19A(H19A)
6.d Idealised Me refined as rotating group:
 C122(H12A,H12B,H12C), C40(H40A,H40B,H40C), C121(H12D,H12E,H12F), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C),
 C1A1(H1AD,H1AE,H1AF), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C41(H41A,
 H41B,H41C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 184 electrons were
found in a volume of 737\%A^3 in 1 void per unit cell.
This is consistent with the presence of 4[CH3CN] per Formula Unit 
which account for 176 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36903
_shelx_fab_checksum              574
_olex2_submission_special_instructions 'No special instructions were received'