A Novel Approach toward Asymmetric Synthesis of Alcohol Functionalized C-Chiral Diphosphines via Two-Stage Hydrophosphination of Terminal Alkynols
Pullarkat, Sumod A.; Yi, Ding; Li, Yongxin; Tan, Geok-Kheng; Leung, Pak-Hing; Inorganic Chemistry 45 (2006) 7455–7463; doi:10.1021/ic060937m

data_4332846
_publ_section_title
;
 A Novel Approach toward Asymmetric Synthesis of Alcohol Functionalized
 C-Chiral Diphosphines via Two-Stage Hydrophosphination of Terminal
 Alkynols
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7455
_journal_page_last               7463
_journal_paper_doi               10.1021/ic060937m
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C41.5 H43 Cl2 N O5 P2 Pd'
_chemical_formula_weight         875.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.5550(10)
_cell_angle_beta                 92.7950(10)
_cell_angle_gamma                98.1280(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7268(4)
_cell_length_b                   10.9351(5)
_cell_length_c                   19.9748(9)
_cell_measurement_reflns_used    3556
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18.85
_cell_measurement_theta_min      2.29
_cell_volume                     2017.83(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21800
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.8701
_exptl_absorpt_correction_type   'SADABS, (Sheldrick 2001)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         14114
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                11283
_reflns_number_total             14114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060937msup3.cif
_cod_data_source_block           3074
_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 
;
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C41.50 H43 Cl2 N O5 P2 Pd'
_cod_database_code               4332846