Syntheses, Structures, and Electronic Interactions of Dicyanamide/Tricyanomethanide-Bridged Binuclear Organometallic Complexes
Li-Yi Zhang; Lin-Xi Shi; Zhong-Ning Chen; Inorganic Chemistry 42 (2003) 633–640; doi:10.1021/ic025879t

data_4312957
_publ_contact_author
;
Zhong-Ning Chen
Fujian Institute of Research on the Structure of Matter, 
Chinese Academy of Sciences, Fuzhou, Fujian 350002, China.
;
_publ_contact_author_email       '  czn@ms.fjirsm.ac.cn '
_publ_section_title
;
 Syntheses, Structures, and Electronic Interactions of
 Dicyanamide/Tricyanomethanide-Bridged Binuclear Organometallic Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              633
_journal_page_last               640
_journal_paper_doi               10.1021/ic025879t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C33.5 H29 F1.5 Fe N1.5 O1.5 P2 S0.5'
_chemical_formula_weight         638.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.3480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4730(2)
_cell_length_b                   18.0376(3)
_cell_length_c                   20.86220(10)
_cell_measurement_reflns_used    4502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      1.68
_cell_volume                     6188.28(13)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9759
_diffrn_reflns_theta_full        24.49
_diffrn_reflns_theta_max         24.49
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .7868
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'polydral pyramid'
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0591P)^2^+29.5727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                3811
_reflns_number_total             5121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025879t-6_s1_6.cif
_cod_data_source_block           6(Compound9CF3SO3)
_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_original_formula_sum        'C33.50 H29 F1.50 Fe N1.50 O1.50 P2 S0.50'
_cod_database_code               4312957