Solvent exchange in a metal‒organic framework single crystal monitored by dynamic <i>in situ</i> X-ray diffraction
Cox, Jordan M.; Walton, Ian M.; Bateman, Gage; Benson, Cassidy A.; Mitchell, Travis; Sylvester, Eric; Chen, Yu-Sheng; Benedict, Jason B.; Acta Crystallographica Section B 73 (2017) 669–674; doi:10.1107/S2052520617008447

data_2108139
_publ_section_title
;
 Solvent exchange in a metal--organic framework single crystal monitored
 by dynamic <i>in situ</i> X-ray diffraction
;
_journal_coeditor_code           LC5089
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              669
_journal_page_last               674
_journal_paper_doi               10.1107/S2052520617008447
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C13 H11 Co N2 O5, 2(H2 O)'
_chemical_formula_sum            'C13 H15 Co N2 O7'
_chemical_formula_weight         370.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.636(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.655(3)
_cell_length_b                   7.6693(19)
_cell_length_c                   15.934(4)
_cell_measurement_reflns_used    1379
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      12.973
_cell_measurement_theta_min      2.530
_cell_volume                     1481.7(6)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40651
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13840
_diffrn_reflns_theta_full        14.753
_diffrn_reflns_theta_max         14.753
_diffrn_reflns_theta_min         1.526
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1112 before and 0.0704 after correction. The Ratio of
minimum to maximum transmission is 0.8584. The \l/2 correction
factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2948
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0550P)^2^+2.0543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                1801
_reflns_number_total             2948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lc5089sup1.cif
_cod_data_source_block           structure1
_cod_database_code               2108139
_cod_database_fobs_code 2108139