Imination reactions of free and coordinated 2-diphenylphosphino-1-phenyl-phospholane: Access to regioisomeric ruthenium(<small>II</small>) complexes containing novel iminophosphorane‒phosphine ligands
Alba E. Díaz-Álvarez; Pascale Crochet; Maria Zablocka; Victorio Cadierno; Carine Duhayon; José Gimeno; Jean-Pierre Majoral; New Journal of Chemistry 30 (2006) 1295–; doi:10.1039/b606781f

data_7052342
_publ_section_title
;
 Imination reactions of free and coordinated
 2-diphenylphosphino-1-phenyl-phospholane: Access to regioisomeric
 ruthenium(<small>II</small>) complexes containing novel
 iminophosphorane--phosphine ligands
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1295
_journal_paper_doi               10.1039/b606781f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety
'C78 H72 Cl2 F8 N4 P4 Ru2, 2(C4 H10 O), 2(F6 Sb) '
_chemical_formula_sum            'C86 H92 Cl2 F20 N4 O2 P4 Ru2 Sb2'
_chemical_formula_weight         2234.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-06-09
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 99.750(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4570(10)
_cell_length_b                   14.6930(8)
_cell_length_c                   20.1840(11)
_cell_measurement_reflns_used    6792
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     4517.8(5)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.113
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39404
_diffrn_reflns_theta_full        29.014
_diffrn_reflns_theta_max         29.014
_diffrn_reflns_theta_min         2.950
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.93
_refine_diff_density_min         -1.91
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1485
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         4864
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1657
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.000550
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
10.9 1.77 8.89 3.38
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0828
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0675
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4864
_reflns_number_total             12075
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            b606781f.txt
_cod_data_source_block           CRYSTALS_cif_3
_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 1 21/c 1 '
_cod_database_code               7052342