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_4317110
_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_sum            'C10 H12 Ni2 O14 S4'
_chemical_formula_weight         601.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.078(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.256(4)
_cell_length_b                   5.3176(10)
_cell_length_c                   18.467(4)
_cell_measurement_reflns_used    1823
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      3.03
_cell_volume                     1890.6(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1198
_diffrn_reflns_av_sigmaI/netI    0.0971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19940
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    2.506
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3362
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0933P)^2^+7.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1833
_reflns_number_gt                2235
_reflns_number_total             3362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101906u_si_001_2.cif
_cod_data_source_block           MIL136Nidehyd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317110