Tuning the Adsorption-Induced Phase Change in the Flexible Metal-Organic Framework Co(bdp).
Taylor, Mercedes K.; Runčevski, Tomče; Oktawiec, Julia; Gonzalez, Miguel I.; Siegelman, Rebecca L.; Mason, Jarad A.; Ye, Jinxing; Brown, Craig M.; Long, Jeffrey R.; Journal of the American Chemical Society 138 (2016) 15019–15026; doi:10.1021/jacs.6b09155

data_4131068
_publ_section_title
;
 Tuning the Adsorption-Induced Phase Change in the Flexible Metal-Organic
 Framework Co(bdp).
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15019
_journal_page_last               15026
_journal_paper_doi               10.1021/jacs.6b09155
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C12 H4 Co D4 N4'
_chemical_formula_sum            'C12 H4 Co D4 N4'
_chemical_formula_weight         271.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2909(5)
_cell_length_b                   13.2909(5)
_cell_length_c                   14.3560(6)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.350
_cell_measurement_theta_min      2.277
_cell_volume                     2535.96(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38643
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.699
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1467 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.9346. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         3051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0480P)^2^+0.2563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2881
_reflns_number_total             3051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09155_si_004.cif
_cod_data_source_block           mkt018s_sq
_cod_original_cell_volume        2536.0(2)
_cod_database_code               4131068
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.69(3) 0.31(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(D4), C5(D5), C8(H8)
;
_shelx_res_checksum              34658
_shelx_hkl_checksum              15202
_shelx_fab_checksum              96288
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'