Solvent- and Pressure-Induced Phase Changes in Two 3D Copper Glutarate-Based Metal-Organic Frameworks via Glutarate (+gauche ⇄ -gauche) Conformational Isomerism.
Bezuidenhout, Charl X.; Smith, Vincent J.; Esterhuysen, Catharine; Barbour, Leonard J.; Journal of the American Chemical Society 139 (2017) 5923–5929; doi:10.1021/jacs.7b01764

data_4125920
_publ_section_title
;
 Solvent- and Pressure-Induced Phase Changes in Two 3D Copper
 Glutarate-Based Metal-Organic Frameworks via Glutarate (+gauche &#x21C4;
 -gauche) Conformational Isomerism.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5923
_journal_page_last               5929
_journal_paper_doi               10.1021/jacs.7b01764
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '0.25(C92 H104 Cu8 N8 O32), 1.61(C O2)'
_chemical_formula_sum            'C24.61 H26 Cu2 N2 O11.23'
_chemical_formula_weight         656.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.255(9)
_cell_length_b                   11.819(4)
_cell_length_c                   9.148(3)
_cell_measurement_reflns_used    2711
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.292
_cell_measurement_theta_min      2.913
_cell_volume                     2946.8(17)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16238
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         1.494
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.9484
_exptl_absorpt_correction_T_min  0.7202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0885 before and 0.0412 after correction.
The Ratio of minimum to maximum transmission is 0.7753.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+2.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2488
_reflns_number_total             3372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2b_prime.cif
_cod_data_source_block           2b_prime
_cod_depositor_comments
'Adding full bibliography for 4125916--4125921.cif.'
_cod_original_cell_volume        2946.6(17)
_cod_database_code               4125920
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) O6(0.59751) O5(0.59751) C7(0.59751) O7(0.41972)
 C14(0.20986)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C1(H1A,H1B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C16(H16), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'