Copper/Zinc-Directed Heterometallic Uranyl-Organic Polycatenating Frameworks: Synthesis, Characterization, and Anion-Dependent Structural Regulation.
Zhao, Ran; Mei, Lei; Wang, Lin; Chai, Zhi-Fang; Shi, Wei-Qun; Inorganic chemistry 55 (2016) 10125–10134; doi:10.1021/acs.inorgchem.6b00786

data_4347927
_publ_section_title
;
 Copper/Zinc-Directed Heterometallic Uranyl-Organic Polycatenating
 Frameworks: Synthesis, Characterization, and Anion-Dependent Structural
 Regulation.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10125
_journal_page_last               10134
_journal_paper_doi               10.1021/acs.inorgchem.6b00786
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C24 H18 N4 O19 S U2 Zn'
_chemical_formula_sum            'C24 H18 N4 O19 S U2 Zn'
_chemical_formula_weight         1239.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_cell_angle_alpha                72.6600(10)
_cell_angle_beta                 83.4470(10)
_cell_angle_gamma                71.3020(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4771(3)
_cell_length_b                   11.4559(4)
_cell_length_c                   15.8438(5)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.323
_cell_measurement_theta_min      6.212
_cell_volume                     1554.98(9)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45962
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.855
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.315
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0611 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.8789.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_refine_diff_density_max         2.552
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0129P)^2^+10.3803P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5276
_reflns_number_total             5682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00786_si_002.cif
_cod_data_source_block           3-Zn
_cod_database_code               4347927
_shelxl_version_number           2013-2
_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
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C9(H9), C7(H7), C15(H15), C10(H10), C13(H13), C22(H22),
 C21(H21), C1(H1), C3(H3), C4(H4)
;
_olex2_submission_original_sample_id 3_Zn
_olex2_submission_special_instructions 'No special instructions were received'