Reinvestigation of the MII (M = Ni, Co)/TetraThiafulvaleneTetraCarboxylate System Using High-Throughput Methods: Isolation of a Molecular Complex and Its Single-Crystal-to-Single-Crystal Transformation to a Two-Dimensional Coordination Polymer
Thi Le Anh Nguyen; Thomas Devic; Pierre Mialane; Eric Rivière; Andreas Sonnauer; Norbert Stock; Rezan Demir-Cakan; Mathieu Morcrette; Carine Livage; Jérome Marrot; Jean-Marie Tarascon; Gérard Férey; Inorganic Chemistry 49 (2010) 10710–10717; doi:10.1021/ic101906u

data_4317111
_publ_section_title
;
 Reinvestigation of the MII (M = Ni,
 Co)/TetraThiafulvaleneTetraCarboxylate System Using High-Throughput
 Methods: Isolation of a Molecular Complex and Its
 Single-Crystal-to-Single-Crystal Transformation to a Two-Dimensional
 Coordination Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10710
_journal_page_last               10717
_journal_paper_doi               10.1021/ic101906u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         C10H24Co2O20S4
_chemical_formula_sum            'C10 H12 Co2 O20 S4'
_chemical_formula_weight         698.29
_chemical_name_common            'Co2(TTF-TC)8H20, 4H2O'
_chemical_name_systematic
;
octa aqueous dicobalt(II)
tetrathiafulvalenetetracarboxylate, water solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.527(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.900(5)
_cell_length_b                   5.0819(18)
_cell_length_c                   17.920(6)
_cell_measurement_reflns_used    1082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      1.82
_cell_volume                     1264.6(8)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3978
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  0.9500
_exptl_absorpt_correction_T_min  0.7817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+2.7089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1964
_reflns_number_gt                1581
_reflns_number_total             2711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101906u_si_001_3.cif
_cod_data_source_block           MIL136Co
_cod_depositor_comments
;

2021-04-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C20 H24 Co4 O40 S8'
_cod_original_formula_weight         1396.59
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1264.6(7)
_cod_database_code               4317111