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_7052340
_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         'C44 H46 Cl2 N O3 P3 Ru, C H Cl3 '
_chemical_formula_sum            'C45 H47 Cl5 N O3 P3 Ru'
_chemical_formula_weight         1021.07
_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             04-11-04
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 95.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.247(4)
_cell_length_b                   10.040(2)
_cell_length_c                   20.632(4)
_cell_measurement_reflns_used    5837
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.7
_cell_volume                     4584.0(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.036
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34425
_diffrn_reflns_theta_full        26.578
_diffrn_reflns_theta_max         26.578
_diffrn_reflns_theta_min         2.739
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             2088.001
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1191
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.018222
_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:
1.77 -0.138 1.28
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0519
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0493
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                4376
_reflns_number_total             9554
_reflns_threshold_expression     I>2.50u(I)
_cod_data_source_file            b606781f.txt
_cod_data_source_block           CRYSTALS_cif
_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_cell_volume        4584.0(16)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C45 H47 Cl5 N1 O3 P3 Ru1'
_cod_database_code               7052340