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_4131072
_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 H6 Co F2 N4'
_chemical_formula_sum            'C12 H6 Co F2 N4'
_chemical_formula_weight         303.14
_chemical_name_common            Co(o-F2-bdp)
_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
_audit_creation_date             2016-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   13.2891(5)
_cell_length_b                   13.2891(5)
_cell_length_c                   43.2262(19)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.595
_cell_measurement_theta_min      2.598
_cell_volume                     7633.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            83198
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        32.097
_diffrn_reflns_theta_max         32.239
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1425 before and 0.0885 after correction.
The Ratio of minimum to maximum transmission is 0.8524.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.836
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6994
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0767P)^2^+5.1288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6096
_reflns_number_total             6994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09155_si_002.cif
_cod_data_source_block           mkt009s_sq
_cod_original_cell_volume        7633.8(7)
_cod_database_code               4131072
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.42(3) 0.58(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 F6-C17 \\sim F5-C16 \\sim F2-C6 \\sim F1-C5 \\sim F3-C8 \\sim F4-C9
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim F3 \\sim F4 \\sim F1
\\sim F2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C15 \\sim C16 \\sim C17 \\sim C18 \\sim F5 \\sim F6: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C8, C9, F3, F4, F1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, C17, C18, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H8)=Sof(H9)=Sof(F1)=Sof(F2)=1-FVAR(1)
 Sof(H5)=Sof(H6)=Sof(F3)=Sof(F4)=FVAR(1)
 Fixed Sof: H16(0.5) H17(0.5) F5(0.5) F6(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C20(H20)
;
_shelx_res_checksum              72874
_shelx_hkl_checksum              50839
_shelx_fab_checksum              81987
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'