Syntheses and Properties of Dinuclear Group 6 Metal Complexes with the Zwitterionic Sulfur Donor Ligand Bis(N,N-diethylamino)carbeniumdithiocarboxylate
Sugaya, Tomoaki; Ohba, Takeshi; Sai, Fumiya; Mashima, Shigeru; Fujihara, Takashi; Unoura, Kei; Nagasawa, Akira; Organometallics 32 (2013) 3441–; doi:10.1021/om300831y

data_4089714
_publ_section_title
;
 Syntheses and Properties of Dinuclear Group 6 Metal Complexes with the
 Zwitterionic Sulfur Donor Ligand
 Bis(N,N-diethylamino)carbeniumdithiocarboxylate
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3441
_journal_paper_doi               10.1021/om300831y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C20 H20 Cr2 N2 O10 S2'
_chemical_formula_weight         616.50
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 102.203(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9141(15)
_cell_length_b                   30.893(5)
_cell_length_c                   10.0997(16)
_cell_measurement_reflns_used    3898
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.34
_cell_volume                     2718.4(8)
_computing_cell_refinement       'SAINT-W2K/NT(Bruker, 2003)'
_computing_data_collection       'SMART-W2K/NT(Bruker, 2003)'
_computing_data_reduction        SAINT-W2K/NT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXTL-NT
_computing_structure_refinement  SHELXTL-NT
_computing_structure_solution    'SHELXTL-NT(Bruker, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18376
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  500
_diffrn_standards_number         113
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                4166
_reflns_number_total             6522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300831y_si_001.cif
_cod_data_source_block           CrEtL
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2718.5(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4089714