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_7040512
_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         'C27 H18 Co2 N O11, C2 H8 N'
_chemical_formula_sum            'C29 H26 Co2 N2 O11'
_chemical_formula_weight         696.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1lj64g
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_audit_update_record
;
2016-08-23 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.582(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.162(2)
_cell_length_b                   15.986(4)
_cell_length_c                   23.971(6)
_cell_measurement_reflns_used    5989
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.215
_cell_measurement_theta_min      2.399
_cell_volume                     3839.8(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23117
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.422
_diffrn_reflns_theta_min         1.538
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.7856.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1295P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6525
_reflns_number_total             9276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02846b2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
;Adding full bibliography for 7040511--7040514.cif.

 Adding full bibliography for 7040511--7040514.cif.
;
_cod_original_cell_volume        3839.6(15)
_cod_database_code               7040512
_olex2_refinement_description
;
1. 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 C(H,H,H,H,H,H) groups
2. Restrained distances
 C24-C25A
 1.5 with sigma of 0.02
 C25-O11
 2.6 with sigma of 0.02
 C28-N2
 1.4 with sigma of 0.02
 N2-C29
 1.4 with sigma of 0.02
 C28-C29
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O11, O11A, N1, N1A, C24, C25, C25A, C26, C26A, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O11A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(O11)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=FVAR(1)
 Sof(N1A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(2)
 Sof(N1)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C27(H27D,H27E,H27F)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), C17(H17), C19(H19),
 C21(H21)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C26(H26A,H26B,H26C), C26A(H26D,
 H26E,H26F), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              64896
_shelx_fab_checksum              61173
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'