An effective strategy to boost the robustness of metal-organic frameworks via introduction of size-matching ligand braces.
Wang, Xiuli; Gao, Wen-Yang; Luan, Jian; Wojtas, Lukasz; Ma, Shengqian; Chemical communications (Cambridge, England) 52 (2016) 1971–1974; doi:10.1039/c5cc09432a

data_7118592
_publ_section_title
;
 An effective strategy to boost the robustness of metal-organic frameworks
 via introduction of size-matching ligand braces.
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1971
_journal_page_last               1974
_journal_paper_doi               10.1039/c5cc09432a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C62 H32 Co3 N3.25 O14, C3 N O0.5, 0.5(C4 N O), C2 N'
_chemical_formula_sum            'C69 H32 Co3 N5.75 O15'
_chemical_formula_weight         1358.29
_chemical_melting_point          ?
_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
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2015-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6069(4)
_cell_length_b                   26.4325(8)
_cell_length_c                   16.6221(5)
_cell_measurement_reflns_used    4235
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      66.88
_cell_measurement_theta_min      3.29
_cell_volume                     6857.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      233.15
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1311
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62684
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.621
_diffrn_reflns_theta_min         4.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.182
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1390 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.4123.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             2749
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12196
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0974P)^2^+10.0378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7836
_reflns_number_total             12196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc09432a2.cif
_cod_data_source_block           xiuli_co8_dma_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7118592
_shelx_estimated_absorpt_t_max   0.500
_shelx_estimated_absorpt_t_min   0.318
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{O92, O91}
3. Restrained distances
 N99-C101 = N99-C100
 1.45 with sigma of 0.02
 N95-C96 = N95-C97
 1.45 with sigma of 0.02
 N103-C102 = N103-C104
 1.45 with sigma of 0.02
 O105-C106
 1.23 with sigma of 0.02
 C115-C116
 1.53 with sigma of 0.01
 N118-C119 = N118-C117
 1.45 with sigma of 0.01
 N118-C115
 1.32 with sigma of 0.01
 C121-N120
 1.4 with sigma of 0.02
 N120-C119
 1.45 with sigma of 0.02
 C97-C98
 1.53 with sigma of 0.02
 N99-C98
 1.32 with sigma of 0.02
 N112-C111 = N112-C113
 1.45 with sigma of 0.02
 C107-C106
 1.53 with sigma of 0.02
 N108-C109 = N108-C110
 1.45 with sigma of 0.02
 O122-C123
 1.23 with sigma of 0.01
 C124-C123
 1.53 with sigma of 0.01
 N126-C127 = N126-C125
 1.45 with sigma of 0.01
 N129-C130
 1.45 with sigma of 0.01
 C128-N129
 1.45 with sigma of 0.01
 O114-C115
 1.23 with sigma of 0.01
 N95-C93
 1.32 with sigma of 0.02
 C94-C93
 1.53 with sigma of 0.02
 O91-C98 = O92-C93
 1.23 with sigma of 0.02
 C96-C97
 2.47 with sigma of 0.04
 C101-C100
 2.47 with sigma of 0.04
 C97-N99
 2.4 with sigma of 0.04
 C94-N95
 2.4 with sigma of 0.04
 C102-C104
 2.47 with sigma of 0.04
 C117-C119
 2.47 with sigma of 0.02
 C117-C115
 2.41 with sigma of 0.02
 C115-C119
 2.41 with sigma of 0.02
 N118-C116
 2.4 with sigma of 0.01
 C100-C98
 2.41 with sigma of 0.04
 C111-C113
 2.47 with sigma of 0.04
 C109-C110
 2.47 with sigma of 0.04
 C110-C106
 2.41 with sigma of 0.04
 C106-C109
 2.41 with sigma of 0.04
 N108-O105
 2.26 with sigma of 0.04
 N108-C107
 2.4 with sigma of 0.02
 O122-C124
 2.43 with sigma of 0.01
 N126-O122
 2.26 with sigma of 0.01
 N126-C124
 2.4 with sigma of 0.01
 C123-C125
 2.41 with sigma of 0.01
 C127-C123
 2.41 with sigma of 0.01
 C127-C125
 2.47 with sigma of 0.01
 C130-C128
 2.47 with sigma of 0.01
 O114-N118
 2.26 with sigma of 0.01
 C93-C97
 2.41 with sigma of 0.04
 C96-C93
 2.41 with sigma of 0.04
 O92-C94
 2.43 with sigma of 0.04
4. Restrained planarity
 O105, C106, C107, N108, C109, C110
 with sigma of 0.1
 O122, C123, C124, C125, N126, C127
 with sigma of 0.1
 O114, C115, C116, C117, N118, C119
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C102 \\sim N103 \\sim C104: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C109 \\sim C113: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N108 \\sim N112: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N126 \\sim O122 \\sim C123 \\sim C124 \\sim C125 \\sim C127 \\sim C128 \\sim
N129 \\sim C130: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N118 \\sim O114 \\sim C115 \\sim C116 \\sim C117 \\sim C119 \\sim N120 \\sim
C121: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O91 \\sim O92 \\sim C93 \\sim C94 \\sim N95 \\sim C96 \\sim C97 \\sim C98 \\sim
N99 \\sim C100 \\sim C101 \\sim C102 \\sim N103 \\sim C104: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O131) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.01
Uiso(O92) = Uiso(O91)
6. Others
 Fixed Sof: O91(0.3) O92(0.2) C93(0.2) C94(0.2) N95(0.2) C96(0.2) C97(0.5)
 C98(0.3) N99(0.3) C100(0.3) C101(0.3) C102(0.5) N103(0.5) C104(0.5) O105(0.5)
 C106(0.25) C107(0.25) N108(0.25) C109(0.25) C110(0.25) O114(0.5) C115(0.5)
 C116(0.5) C117(0.5) N118(0.5) N120(0.5) C121(0.5) O122(0.5) C123(0.5)
 C124(0.5) C125(0.5) N126(0.5) C127(0.5) C128(0.5) N129(0.5) C130(0.5)
 C111(0.5) N112(0.5) C113(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21),
 C22(H22), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48),
  C49(H49), C54(H54), C55(H55), C59(H59), C60(H60), C67(H67), C68(H68),
 C69(H69), C70(H70), C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C79(H79),
  C81(H81), C82(H82)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'