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_4125916
_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(C88 H96 Cu8 N8 O32)'
_chemical_formula_sum            'C22 H24 Cu2 N2 O8'
_chemical_formula_weight         571.51
_chemical_name_systematic        '[Cu2glu2Bpa]n'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 91.627(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4258(11)
_cell_length_b                   13.1097(6)
_cell_length_c                   8.6242(4)
_cell_measurement_reflns_used    6941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.93
_cell_volume                     2760.5(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10270
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.668
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1266 before and 0.0557 after correction. The Ratio of minimum to maximum transmission is 0.6623. The \l/2 correction factor is 0.0000.'
_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    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.542
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0197P)^2^+7.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2229
_reflns_number_total             2341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1a.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4125916--4125921.cif.'
_cod_database_code               4125916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.481
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9A) = Uanis(C9B)
Uanis(N1A) = Uanis(N1B)
Uanis(C11A) = Uanis(C8A) = Uanis(C8B) = Uanis(C7B) = Uanis(C7A) = Uanis(C10B) =
Uanis(C10A) = Uanis(C6B) = Uanis(C6A) = Uanis(C11B)
3. Others
 Sof(H9BA)=Sof(H9BB)=Sof(H7B)=Sof(H10B)=Sof(H11B)=Sof(H6B)=1-FVAR(1)
 Sof(H6A)=Sof(H7A)=Sof(H11A)=Sof(H10A)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Fixed Sof: N1B(0.20843) C6A(0.79157) C7A(0.79157) C8A(0.79157) C11A(0.79157)
 C10A(0.79157) C9A(0.79157) C9B(0.20843) C8B(0.20843) C7B(0.20843)
 C10B(0.20843) C11B(0.20843) C6B(0.20843) N1A(0.79157)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C9A(H9AA,H9AB), C2(H2A,H2B), C9B(H9BA,H9BB)
4.b Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C7A(H7A), C11A(H11A), C10A(H10A), C7B(H7B), C10B(H10B), C11B(H11B),
 C6B(H6B)
;
_olex2_submission_special_instructions 'No special instructions were received'