Influence of Metal Substitution on the Pressure-Induced Phase Change in Flexible Zeolitic Imidazolate Frameworks.
McGuirk, C. Michael; Runčevski, Tomče; Oktawiec, Julia; Turkiewicz, Ari; Taylor, Mercedes K.; Long, Jeffrey R.; Journal of the American Chemical Society 140 (2018) 15924–15933; doi:10.1021/jacs.8b09631

data_4133329
_publ_section_title
;
 Influence of Metal Substitution on the Pressure-Induced Phase Change in
 Flexible Zeolitic Imidazolate Frameworks.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15924
_journal_page_last               15933
_journal_paper_doi               10.1021/jacs.8b09631
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C336 H240 Cd24 N96, 26(C3 H7 N O)'
_chemical_formula_sum            'C414 H422 Cd24 N122 O26'
_chemical_formula_weight         10220.31
_chemical_name_common            'CdIF-13 DMF-solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.639(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   16.2363(6)
_cell_length_b                   22.6153(10)
_cell_length_c                   29.9087(12)
_cell_measurement_reflns_used    9533
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.496
_cell_measurement_theta_min      2.329
_cell_volume                     10946.2(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            172937
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         1.401
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.8655.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             5120
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.711
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         22032
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0490P)^2^+74.0282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17526
_reflns_number_total             22032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09631_si_002.cif
_cod_data_source_block           cmm060s_sq
_cod_database_code               4133329
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C102-N30 \\sim C100-N30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim N27 \\sim C91 \\sim C92 \\sim C93: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O5 \\sim N29 \\sim C97 \\sim C98 \\sim C99: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O6 \\sim N30 \\sim C100 \\sim C101 \\sim C102: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O3, N27, C91, C92, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N29, C97, C98, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, N30, C100, C101, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O6(0.5) N30(0.5) C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C101(0.5)
 H101(0.5) C102(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C67(H67),
  C68(H68), C69(H69), C70(H70), C71(H71), C74(H74), C75(H75), C76(H76),
 C77(H77), C78(H78), C81(H81), C82(H82), C83(H83), C84(H84), C93(H93), C96(H96),
  C87(H87), C99(H99), C101(H101), C90(H90)
6.b Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C97(H97A,H97B,H97C), C98(H98A,
 H98B,H98C), C100(H10A,H10B,H10C), C102(H10D,H10E,H10F), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C)
;
_shelx_fab_checksum              4891
_olex2_submission_special_instructions 'No special instructions were received'