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_7118593
_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         '0.5(C120 H48 Co6 N6 O32), 2(C2 N1), 2.76(O)'
_chemical_formula_sum            'C64 H24 Co3 N5 O18.75'
_chemical_formula_weight         1339.75
_chemical_melting_point          ?
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.3816(3)
_cell_length_b                   15.3816(3)
_cell_length_c                   16.8215(4)
_cell_measurement_reflns_used    3191
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      65.07
_cell_measurement_theta_min      3.32
_cell_volume                     3446.66(13)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      233.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0693
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_laue_measured_fraction_full 0.974
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15678
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        66.505
_diffrn_reflns_theta_max         66.505
_diffrn_reflns_theta_min         3.318
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.182
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1406 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.4867.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1982
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1624
_reflns_number_total             1982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc09432a2.cif
_cod_data_source_block           wy_nano_co_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_original_cell_volume        3446.66(16)
_cod_database_code               7118593
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{O13, O14}
3. Restrained distances
 N24-C25 = N24-C23
 1.48 with sigma of 0.02
 O13-C14 = C18-O14
 1.23 with sigma of 0.02
 N20-C22 = N20-C26
 1.45 with sigma of 0.02
 C19-C18 = C14-C21
 1.53 with sigma of 0.01
 N15-C23 = N15-C25
 1.45 with sigma of 0.02
 N20-C18 = C14-N15
 1.32 with sigma of 0.02
 C17-C16 = C22-C26 = C23-C25
 2.47 with sigma of 0.04
 C22-C18 = C17-C14 = C26-C18 = C16-C14
 2.43 with sigma of 0.04
 N20-C19 = N15-C21
 2.4 with sigma of 0.02
4. Restrained planarity
 C22, N20, C26, C18, O13, C19
 with sigma of 0.1
 O14, C14, C17, N15, C16
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C14 \\sim N15 \\sim C18 \\sim N20 \\sim C21 \\sim N24 \\sim C25 \\sim C16 \\sim
C19 \\sim C17 \\sim C22 \\sim C23 \\sim O13 \\sim C26: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(O13) = Uanis(O14)
6. Others
 Fixed Sof: O13(0.3) C14(0.3) N15(0.3) C16(0.3) C17(0.3) C18(0.2) C19(0.2)
 N20(0.2) O14(0.2) C21(0.3) C22(0.2) C23(0.3333) N24(0.3333) C25(0.3333)
 O31(0.0835) O32(0.0835) O33(0.0835) O34(0.0835) O35(0.0835) O36(0.02783)
 O37(0.01392) C26(0.2)
7.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C11(H11), C12(H12)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'