Synthesis and Structure Determinations of Complexes Containing a Five-Membered Lactam Structure Based on Organohydrazido(2-) Ligands1
Hidetake Seino; Youichi Ishii; Masanobu Hidai; Inorganic Chemistry 36 (1997) 161–171; doi:10.1021/ic960778e

data_4323287
_publ_contact_author
;
   Hidai, Masanobu
   Department of Chemistry and Biotechnology, Graduate School of Engineering,
   the University of Tokyo, Tokyo, Hongo, Bunkyo-ku 113, Japan
;
_publ_contact_author_fax         ' +81 3-(5800)-6945 '
_publ_section_title
;
 Synthesis and Structure Determinations of Complexes Containing a
 Five-Membered Lactam Structure Based on Organohydrazido(2-) Ligands1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              161
_journal_page_last               171
_journal_paper_doi               10.1021/ic960778e
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C35 H42 Cl2 N2 O P3 W'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Wed Jun 19 09:28:28 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.97(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8.00
_cell_length_a                   37.952(4)
_cell_length_b                   18.382(3)
_cell_length_c                   10.368(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      41.82
_cell_measurement_theta_min      38.64
_cell_volume                     7216(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.01413
_diffrn_orient_matrix_UB_12      0.04545
_diffrn_orient_matrix_UB_13      0.01575
_diffrn_orient_matrix_UB_21      -0.02199
_diffrn_orient_matrix_UB_22      0.02973
_diffrn_orient_matrix_UB_23      -0.01417
_diffrn_orient_matrix_UB_31      -0.00379
_diffrn_orient_matrix_UB_32      -0.00312
_diffrn_orient_matrix_UB_33      0.09433
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            8660
_diffrn_reflns_theta_max         27.4971
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        -0.04
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 35.164
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      1.548
_exptl_crystal_density_meas_temp 290
_exptl_crystal_density_method    flotation
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416.00
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         -2.26540
_refine_diff_density_min         1.45540
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.690
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5062
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0540
_refine_ls_shift/esd_max         0.1460
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0460
_cod_data_source_file            ic960778e_1.cif
_cod_data_source_block
'[WCl2(NNCH2C6H4CO)(PMe2Ph)3].0.5C6H6_(3a.0.5C6H6)'
_cod_original_cell_volume        7215(1)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C35 H42 W Cl2 N2 O P3'
_cod_database_code               4323287