Ruthenium Tris(pyrazolyl)borate Diazo Complexes: Preparation of Aryldiazenido, Aryldiazene, and Hydrazine Derivatives
Gabriele Albertin; Stefano Antoniutti; Marco Bortoluzzi; Jesus Castro-Fojo; Soledad García-Fontán; Inorganic Chemistry 43 (2004) 4511–4522; doi:10.1021/ic0497275

data_4311256
_publ_contact_author_address
; Departamento de Qu\'imica Inorg\'anica
  Facultade de Qu\'imica
  Universidade de Vigo
  36200 Vigo
  Galicia, Spain
;
_publ_contact_author_email       fojo@uvigo.es
_publ_contact_author_fax         '0034 986 813798'
_publ_contact_author_name        'Dr. Jes\'us A. Castro'
_publ_contact_author_phone       '0034 986 812278'
_publ_section_title
;
 Ruthenium Tris(pyrazolyl)borate Diazo Complexes: Preparation of
 Aryldiazenido, Aryldiazene, and Hydrazine Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4511
_journal_page_last               4522
_journal_paper_doi               10.1021/ic0497275
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C34 H46 B N8 O3 P2 Ru, C24 H20 B'
_chemical_formula_sum            'C58 H66 B2 N8 O3 P2 Ru'
_chemical_formula_weight         2215.64
_space_group_IT_number           61
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.2119(19)
_cell_length_b                   27.294(4)
_cell_length_c                   29.490(4)
_cell_measurement_temperature    293(2)
_cell_volume                     11439(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1685
_diffrn_reflns_av_sigmaI/netI    0.4325
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            54280
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.786308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.680
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         13531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.680
_refine_ls_R_factor_all          0.3060
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                3267
_reflns_number_total             13531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497275si20040303_064756.cif
_cod_data_source_block           md
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4311256