Four new 3D metal-organic frameworks constructed by the asymmetrical pentacarboxylate: gas sorption behaviour and magnetic properties.
Yan, Yang-Tian; Zhang, Wen-Yan; Wu, Yun-Long; Li, Jiang; Xi, Zheng-Ping; Wang, Yao-Yu; Hou, Lei; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15473–15480; doi:10.1039/c6dt02846b

data_7040513
_publ_section_title
;
 Four new 3D metal-organic frameworks constructed by the asymmetrical
 pentacarboxylate: gas sorption behaviour and magnetic properties.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15473
_journal_page_last               15480
_journal_paper_doi               10.1039/c6dt02846b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C23 H11 Co2 O11, C2 H8 N'
_chemical_formula_sum            'C25 H19 Co2 N O11'
_chemical_formula_weight         627.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1lj65h
_audit_creation_date             2016-08-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.19 svn.r3327 for OlexSys, GUI svn.r5215)
;
_audit_update_record
;
2016-08-23 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.048(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.230(3)
_cell_length_b                   9.468(3)
_cell_length_c                   28.006(9)
_cell_measurement_reflns_used    2575
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.390
_cell_measurement_theta_min      2.945
_cell_volume                     2685.9(14)
_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      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13919
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         1.469
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0740 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.8611.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5101
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1926P)^2^+25.5291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2758
_refine_ls_wR_factor_ref         0.3105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3992
_reflns_number_total             5101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02846b2.cif
_cod_data_source_block           3_sq
_cod_depositor_comments
;Adding full bibliography for 7040511--7040514.cif.

 Adding full bibliography for 7040511--7040514.cif.
;
_cod_original_cell_volume        2685.8(16)
_cod_database_code               7040513
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.908(2) 0.092(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 N1, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 O11(H11A,H11B)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C12(H12), C14(H14), C17(H17), C19(H19),
 C21(H21)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              63562
_shelx_fab_checksum              37701
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'