Complexes of the (1R)-(+)-camphor azine diphosphines Z,Z-3,3′-Ph2PnC10H15N–NC10H15PxPh2 and Z,Z-3,3′-Ph2PxC10H15N–N C10H15PxPh2 (x = exo, n = endo) with Group 6 metal carbonyls: crystal structures of the ligands and fac-[W(CO)3(E,Z-Ph2PxC10H15 N–NC10H15PxPh2)]
Shaw, Bernard L.; Iranpoor, Nasser; Perera, Sarath D.; Thornton-Pett, Mark; Vessey, Jonathan D.; Journal of the Chemical Society, Dalton Transactions  (1998) 1885–; doi:10.1039/a801585f

data_7028085
_publ_section_title
;
 Complexes of the (1R)-(+)-camphor azine diphosphines
 Z,Z-3,3&#x2032;-Ph2PnC10H15&#xE006;N--N&#xE006;C10H15PxPh2 and
 Z,Z-3,3&#x2032;-Ph2PxC10H15&#xE006;N--N&#xE006; C10H15PxPh2
 (x&#x2005;=&#x2005;exo, n&#x2005;=&#x2005;endo) with Group 6 metal
 carbonyls: crystal structures of the ligands and
 fac-[W(CO)3(E,Z-Ph2PxC10H15&#xE006; N--N&#xE006;C10H15PxPh2)]
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_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1885
_journal_paper_doi               10.1039/a801585f
_journal_year                    1998
_chemical_formula_sum            'C44 H50 N2 P2'
_chemical_formula_weight         668.80
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.882(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9559(12)
_cell_length_b                   6.6755(4)
_cell_length_c                   24.0682(12)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      40.0
_cell_measurement_theta_min      35.0
_cell_volume                     3736.5(4)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Stoe STADI4'
_diffrn_measurement_method       \w-\q-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            4091
_diffrn_reflns_theta_max         64.63
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.00068(6)
_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   1.057
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.078
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_obs          0.0287
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+1.4127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0792
_refine_ls_wR_factor_obs         0.0775
_reflns_number_observed          3559
_reflns_number_total             3832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f801585sup1.cif
_cod_data_source_block           nasser1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+1.4127P] 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^)+(0.0423P)^2^+1.4127P] 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        3736.5(3)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7028085