Ionothermal synthesis and structural transformation targeted by ion exchange in metal-1,3,5-benzenetricarboxylate compounds
Xu, Qing-Qing; Liu, Bing; Xu, Ling; Jiao, Huan; Journal of Solid State Chemistry 247 (2017) 1–7; doi:10.1016/j.jssc.2016.12.006

data_1560608
_publ_section_title
;
 Ionothermal synthesis and structural transformation targeted by ion
 exchange in metal-1,3,5-benzenetricarboxylate compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               7
_journal_paper_doi               10.1016/j.jssc.2016.12.006
_journal_volume                  247
_journal_year                    2017
_chemical_formula_moiety         '0.5(C18 H22 Cl2 Cu4 O20)'
_chemical_formula_sum            'C9 H11 Cl Cu2 O10'
_chemical_formula_weight         441.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3641(11)
_cell_length_b                   14.1462(11)
_cell_length_c                   7.4643(6)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.88
_cell_volume                     1516.7(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_molecular_graphics    'Siemens SHELXTL^TM^ 5'
_computing_publication_material  'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18093
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'rotating-anode generator'
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (CrystalClear)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+4.8854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                688
_reflns_number_total             746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mmc7.CIF
_cod_data_source_block           comp3
_cod_database_code               1560608
_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. Rigid bond restraints
 Cu1, O1W
 with sigma for 1-2 distances of 0.4 and sigma for 1-3 distances of 0.2
3.a Rotating group:
 O1W(H1Wa,H1Wb)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12)
;