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_4323359
_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(NH2NH2)[PPh(OEt)2]2}BPh4
;
_chemical_formula_sum            'C47 H54 B M N3 O7 P2'
_chemical_formula_weight         886.65
_chemical_melting_point          392
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'partly difmap and partly calculated'
_atom_sites_solution_primary     direct
_cell_angle_alpha                104.47(1)
_cell_angle_beta                 100.32(1)
_cell_angle_gamma                111.08(1)
_cell_formula_units_Z            2.00
_cell_length_a                   13.772(3)
_cell_length_b                   14.951(4)
_cell_length_c                   13.319(3)
_cell_measurement_radiation      MoK\a
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295
_cell_measurement_theta_max      9.93
_cell_measurement_theta_min      4.5
_cell_measurement_wavelength     0.71069
_cell_volume                     2365.4(10)
_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_radiation_detector       'scintillation counter'
_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  0.12
_diffrn_reflns_av_sigmaI/netI    0.04
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13445
_diffrn_reflns_reduction_process
;
Lorentz and polarization correction
;
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3
_exptl_absorpt_coefficient_mu    0.3963
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.2449
_exptl_crystal_description
;
regular prisms
;
_exptl_crystal_F_000             932.0
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.63
_refine_diff_density_rms         0.07
_refine_ls_goodness_of_fit_all   1.024
_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     561
_refine_ls_number_reflns         13445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.094
_refine_ls_R_factor_obs          0.0511
_refine_ls_shift/esd_max         0.07
_refine_ls_shift/esd_mean        0.01
_refine_ls_structure_factor_coef Fsquare
_refine_ls_weighting_scheme      'according to SHELXL-93 (a=0.1, b=0.18)'
_refine_ls_wR_factor_all         0.1730
_reflns_number_observed          8208
_reflns_number_total             13570
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9608612_2.cif
_cod_data_source_block           Compound-11a
_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_cell_volume        2365(1)
_cod_original_sg_symbol_H-M      ' P -1'
_cod_original_formula_sum        'C47 H54 B MN N2 O7 P2'
_cod_database_code               4323359