Syntheses and structural characterizations of phenylimidorhenium(V) complexes containing bi- or tetra-dentate phosphinoamido ligands
Refosco, Fiorenzo; Bolzati, Cristina; Tisato, Francesco; Bandoli, Giuliano; Journal of the Chemical Society, Dalton Transactions  (1998) 923–; doi:10.1039/a707330e

data_7028031
_publ_section_title
;
 Syntheses and structural characterizations of phenylimidorhenium(V)
 complexes containing bi- or tetra-dentate phosphinoamido ligands
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              923
_journal_paper_doi               10.1039/a707330e
_journal_year                    1998
_chemical_formula_sum            'C47 H45 N3 O1.5 P2 Re'
_chemical_formula_weight         924.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                88.64(3)
_cell_angle_beta                 80.65(3)
_cell_angle_gamma                79.48(3)
_cell_formula_units_Z            4
_cell_length_a                   11.307(4)
_cell_length_b                   13.333(6)
_cell_length_c                   27.743(11)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     4057(3)
_computing_cell_refinement       'P3 diffractometer software'
_computing_data_collection       'P3 diffractometer software'
_computing_data_reduction        'P3 diffractometer software'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-Nicolet R3m/V'
_diffrn_measurement_method       '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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9106
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   'empirical (XEMP in SHELXTL/PC)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.292
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.0000(2)
_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_all   1.321
_refine_ls_goodness_of_fit_obs   1.304
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.322
_refine_ls_restrained_S_obs      1.304
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_obs          0.0505
_refine_ls_shift/esd_max         -6.111
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1642
_refine_ls_wR_factor_obs         0.1452
_reflns_number_observed          7612
_reflns_number_total             9099
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e707330sup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4057.4(28)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C47 H45 N3 O1.50 P2 Re'
_cod_database_code               7028031