Chelated Hydrazido(3-)rhenium(V) Complexes: On the Way to the Nitrido-M(V) Core (M = Tc, Re)
Franck Mévellec; Nicolas Lepareur; Alain Roucoux; Nicolas Noiret; Henri Patin; Giuliano Bandoli; Marina Porchia; Francesco Tisato; Inorganic Chemistry 41 (2002) 1591–1597; doi:10.1021/ic0110979

data_4317737
_publ_section_title
;
 Chelated Hydrazido(3-)rhenium(V) Complexes: On the Way to the
 Nitrido-M(V) Core (M = Tc, Re)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1591
_journal_page_last               1597
_journal_paper_doi               10.1021/ic0110979
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H29 N4 O P Re S4'
_chemical_formula_weight         806.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.33(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.916(3)
_cell_length_b                   10.236(4)
_cell_length_c                   29.463(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      8.1
_cell_volume                     6303(3)
_computing_cell_refinement       'CAD-4 software Ver.5.Enraf-Nonius,Delft, 1989'
_computing_data_collection       'CAD-4 software Ver.5.Enraf-Nonius,Delft, 1989'
_computing_data_reduction        'CAD-4 software Ver.5.Enraf-Nonius,Delft, 1989'
_computing_molecular_graphics    'SHELXTL NT Ver.5.10, Bruker, 1999'
_computing_publication_material  'SHELXTL NT Ver.5.10, Bruker, 1999'
_computing_structure_refinement  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT Ver.5.10, Bruker, 1999'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14094
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.203
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.000000(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         13717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          1.852
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                8713
_reflns_number_total             13717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110979_1.cif
_cod_data_source_block           renio_compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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               4317737