Reaction Products of W(CO)6 with Formamidines; Electronic Structure of a W2(μ-CO)2 Core with Unsymmetric Bridging Carbonyls
F. Albert Cotton; James P. Donahue; Michael B. Hall; Carlos A. Murillo; Dino Villagrán; Inorganic Chemistry 43 (2004) 6954–6964; doi:10.1021/ic049116c

data_4311885
_publ_contact_author_phone       979-845-4432
_publ_section_title
;
 Reaction Products of W(CO)6 with Formamidines; Electronic Structure of a
 W2(\m-CO)2 Core with Unsymmetric Bridging Carbonyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6954
_journal_page_last               6964
_journal_paper_doi               10.1021/ic049116c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(C6 Cl2 H3) N H C O H'
_chemical_formula_sum            'C7 H5 Cl2 N O'
_chemical_formula_weight         190.02
_chemical_melting_point          ?
_chemical_name_systematic        N-(3,5-dichlorophenyl)-formamide
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 109.526(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9426(12)
_cell_length_b                   14.724(2)
_cell_length_c                   7.2916(11)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.77
_cell_volume                     803.7(2)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V. 5.618'
_computing_data_reduction        'SAINT V. 6.22'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2716
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.77
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1605
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0796P)^2^+0.4201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                1466
_reflns_number_total             1605
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic049116csi20040706_041210_1.cif
_cod_data_source_block           N-(3,5-dichlorophenyl)-formamide
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (16
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (24 times).

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:
data name '_publ_contact_author-phone' replaced with
'_publ_contact_author_phone' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4311885