Synthesis and characterization of novel phosphinoketone and phosphinoenolato rhenium(v) nitrido complexes. Crystal structure of ReNCl2{iPr2PCH2C(Ph)O}2
Couillens, Xavier; Gressier, Marie; Dartiguenave, Michèle; Fortin, Sébastien; Beauchamp, André L.; Journal of the Chemical Society, Dalton Transactions  (2002) 3032–; doi:10.1039/b201632j

data_7011568
_publ_section_title
;
 Synthesis and characterization of novel phosphinoketone and
 phosphinoenolato rhenium(v) nitrido complexes. Crystal structure of
 ReNCl2{iPr2PCH2C(Ph)&#xE001;O}2
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3032
_journal_paper_doi               10.1039/b201632j
_journal_year                    2002
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C30 H47 Cl2 N O2.50 P2 Re'
_chemical_formula_sum            'C30 H47 Cl2 N O2.5 P2 Re'
_chemical_formula_weight         780.77
_chemical_name_systematic
; 
? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL96  (Sheldrick, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.27(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.786(10)
_cell_length_b                   9.637(6)
_cell_length_c                   19.444(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      22.00
_cell_measurement_theta_min      20.00
_cell_volume                     3452(4)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRC-2, NRC-2A (Ahmed et al, 1973)'
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus xray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.041
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26423
_diffrn_reflns_theta_max         69.83
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    9.398
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.161
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            'translucent orange-red'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1572.0
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00019(2)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL96 (Sheldrick, 1996)'
_refine_ls_goodness_of_fit_all   0.952
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6545
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.278
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0791
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5440
_reflns_number_total             6545
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b201632j.txt
_cod_data_source_block           seba26
_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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C30 H47 Cl2 N O2.50 P2 Re'
_cod_database_code               7011568