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_1560606
_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         'C40 H48 N8 Ni4 O36, 6(H2 O)'
_chemical_formula_sum            'C40 H60 N8 Ni4 O42'
_chemical_formula_weight         1559.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_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            8
_cell_length_a                   14.4277(5)
_cell_length_b                   24.0577(5)
_cell_length_c                   33.9348(9)
_cell_measurement_reflns_used    5679
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      3.4210
_cell_measurement_theta_min      28.8080
_cell_volume                     11778.7(6)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            14552
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'rotating-anode generator'
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (CrystalClear)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6432
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0685P)^2^+63.8858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                2196
_reflns_number_total             2574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mmc5.CIF
_cod_data_source_block           comp1
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1560606
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O3W(H3WA,H3WB)
3.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C22(H22), C24(H24)
3.d Tetrahedral OH refined with riding coordinates:
 O23(H23A)
3.e X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;