Aryldiazene, Aryldiazenido, and Hydrazine Complexes of Manganese. Preparation, Characterization, and X-ray Crystal Structures of [Mn(CO)3(4-CH3C6H4NNH){PPh(OEt)2}2]BF4 and [Mn(CO)3(NH2NH2){PPh(OEt)2}2]BPh4 Derivatives
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Emilio Bordignon; Fabio Busatto; Giancarlo Pelizzi; Inorganic Chemistry 36 (1997) 1296–1305; doi:10.1021/ic9608612

data_4323358
_publ_section_title
;
 Aryldiazene, Aryldiazenido, and Hydrazine Complexes of Manganese.
 Preparation, Characterization, and X-ray Crystal Structures of
 [Mn(CO)3(4-CH3C6H4NNH){PPh(OEt)2}2]BF4 and
 [Mn(CO)3(NH2NH2){PPh(OEt)2}2]BPh4 Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1296
_journal_page_last               1305
_journal_paper_doi               10.1021/ic9608612
_journal_volume                  36
_journal_year                    1997
_chemical_formula_structural
;
{Mn(CO)3(4-CH3-C6H4-N=NH)[PPh(OEt)2]2}BF4
;
_chemical_formula_sum            'C30 H38 B F4 M N3 O7 P2'
_chemical_formula_weight         742.33
_chemical_melting_point          396
_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   'partly difmap and partly calculated'
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 97.82(1)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            8.00
_cell_length_a                   31.857(5)
_cell_length_b                   11.119(2)
_cell_length_c                   22.414(3)
_cell_measurement_radiation      MoK\a
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.1
_cell_measurement_theta_min      4.8
_cell_measurement_wavelength     0.71069
_cell_volume                     7866(2)
_computing_molecular_graphics    'ZORTEP (Zsolnai, Pritzkow, 1994)'
_computing_publication_material
;
 PARST95 (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_detector       'scintillation tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.06
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8028
_diffrn_reflns_reduction_process
;
Lorentz and polarization
;
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  6000
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.4768
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.2537
_exptl_crystal_description
;
irregular prisms
;
_exptl_crystal_F_000             3072.0
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.09
_refine_ls_goodness_of_fit_all   1.98
_refine_ls_hydrogen_treatment
;
H atoms located on difmap were refined isotropically, those introduced
in calculated positions were readjusted according to the geometry
of the carrier atoms (riding refinement)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.22
_refine_ls_R_factor_obs          0.0708
_refine_ls_shift/esd_max         0.05
_refine_ls_shift/esd_mean        0.02
_refine_ls_structure_factor_coef Fsquare
_refine_ls_weighting_scheme      'according to SHELXL-93 (a=0.1)'
_refine_ls_wR_factor_all         0.36
_reflns_number_observed          3388
_reflns_number_total             8444
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9608612_1.cif
_cod_data_source_block           Compound-1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C30 H38 B F4 MN N2 O7 P2'
_cod_database_code               4323358