Solvent-Induced Single Crystal-Single Crystal Transformation of an Interpenetrated Three-Dimensional Copper Triazole Catalytic Framework.
Wang, Ying; Meng, Shan-Shan; Lin, Peng-Xiang; Xiao, Yi-Wei; Ma, Qing-Qing; Xie, Qiong; Chen, Yuan-Yuan; Zhao, Xiao-Jun; Chen, Jun; Inorganic chemistry 55 (2016) 4069–4071; doi:10.1021/acs.inorgchem.6b00433

data_4347657
_publ_section_title
;
 Solvent-Induced Single Crystal-Single Crystal Transformation of an
 Interpenetrated Three-Dimensional Copper Triazole Catalytic Framework.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4069
_journal_page_last               4071
_journal_paper_doi               10.1021/acs.inorgchem.6b00433
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'0.25(C144 H112 Cu4 N48 O8), 2(N O3), 8(H2 O)'
_chemical_formula_sum            'C36 H44 Cu N14 O16'
_chemical_formula_weight         992.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.08450(19)
_cell_length_b                   14.08450(19)
_cell_length_c                   44.2036(10)
_cell_measurement_reflns_used    5906
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.7320
_cell_measurement_theta_min      4.3350
_cell_volume                     8768.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    6.00   63.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -       55.2238  -77.0000  -90.0000 57

  2 omega   18.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 26

  3 omega   21.00   48.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 27

  4 omega    1.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 25

  5 omega   24.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477  -38.0000  -90.0000 28

  6 omega   40.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477  -25.0000 -150.0000 38

  7 omega  103.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477  111.0000  -90.0000 64

  8 omega  107.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477  111.0000 -180.0000 71

  9 omega   31.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477 -111.0000  150.0000 26

 10 omega   85.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4477 -111.0000  150.0000 30

 11 omega -124.00  -91.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -55.2238  -99.0000 -150.0000 33

 12 omega -146.00  -89.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -55.2238  -99.0000  -60.0000 57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0959806000
_diffrn_orient_matrix_UB_12      -0.0067206000
_diffrn_orient_matrix_UB_13      0.0166112000
_diffrn_orient_matrix_UB_21      -0.0499375000
_diffrn_orient_matrix_UB_22      0.0219137000
_diffrn_orient_matrix_UB_23      0.0302223000
_diffrn_orient_matrix_UB_31      -0.0163768000
_diffrn_orient_matrix_UB_32      -0.1068376000
_diffrn_orient_matrix_UB_33      0.0051440000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            8184
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         4.000
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0541P)^2^+17.0425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3625
_reflns_number_total             3919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00433_si_001.cif
_cod_data_source_block           a150512d
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4347657
_chemical_oxdiff_formula         'C H O N S Zn'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim N7: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O7(H7A,H7B), O6(H6A,H6B), O5(H5A,H5B), O8(H8A,H8B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-05-12
_olex2_submission_special_instructions 'No special instructions were received'