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_4323290
_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            'C57.5 H54 B Br Cl F5 N2 O2 P4 W'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Wed Jun 19 09:30:52 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 109.787(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   12.798(2)
_cell_length_b                   27.619(2)
_cell_length_c                   17.002(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      39.99
_cell_measurement_theta_min      39.33
_cell_volume                     5654.8(12)
_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 scans'
_diffrn_orient_matrix_UB_11      0.04098
_diffrn_orient_matrix_UB_12      -0.02607
_diffrn_orient_matrix_UB_13      -0.01824
_diffrn_orient_matrix_UB_21      0.04195
_diffrn_orient_matrix_UB_22      0.02512
_diffrn_orient_matrix_UB_23      -0.01950
_diffrn_orient_matrix_UB_31      0.05879
_diffrn_orient_matrix_UB_32      0.00025
_diffrn_orient_matrix_UB_33      0.05652
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.29
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            13778
_diffrn_reflns_theta_max         27.4980
_diffrn_reflns_theta_min         4.05
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 29.738
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      1.589
_exptl_crystal_density_meas_temp 290
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2660.00
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
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_refine_diff_density_max         -1.54810
_refine_diff_density_min         2.15090
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.470
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     680
_refine_ls_number_reflns         7862
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         3.3160
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0330
_cod_data_source_file            ic960778e_4.cif
_cod_data_source_block
'[WF{NNCH(OMe)CH=CBrCO}(dppe)2][BF4].0.5CH2Cl2_(18+BF4-)'
_cod_original_cell_volume        5655(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C57.5 H54 W N2 O2 P4 F5 Cl Br B'
_cod_database_code               4323290