Desolvation process in the flexible metal‒organic framework [Cu(Me-4py-trz-ia)], adsorption of dihydrogen and related structure responses
Erhart, Oliver; Georgiev, Peter A.; Krautscheid, Harald; CrystEngComm 21 (2019) 6523–; doi:10.1039/C9CE00992B

data_7233762
_publ_section_title
;
 Desolvation process in the flexible metal--organic framework
 [Cu(Me-4py-trz-ia)], adsorption of dihydrogen and related structure
 responses
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6523
_journal_paper_doi               10.1039/C9CE00992B
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C16 H12 Cu N4 O5'
_chemical_formula_weight         403.84
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-22 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.199(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8663(4)
_cell_length_b                   13.2350(4)
_cell_length_c                   15.0241(4)
_cell_measurement_reflns_used    6154
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      70.83
_cell_measurement_theta_min      4.43
_cell_volume                     2752.93(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29057
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         4.455
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  0.7400
_exptl_absorpt_correction_T_min  0.1964
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, 
Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0556
_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^)+(0.1085P)^2^+1.2647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3605
_reflns_number_total             5133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00992b2.cif
_cod_data_source_block           phase-1b
_cod_depositor_comments
'Adding full bibliography for 7233759--7233763.cif.'
_cod_database_code               7233762
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              59043
_shelx_fab_checksum              79702