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_4332845
_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            'C43 H46 Cl3 N O5 P2 Pd'
_chemical_formula_weight         931.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0929(11)
_cell_length_b                   19.017(2)
_cell_length_c                   22.489(2)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.90
_cell_measurement_theta_min      2.21
_cell_volume                     4316.5(8)
_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      223(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
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_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30270
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_correction_T_min  0.7579
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.825
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9895
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_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0724P)^2^+1.9053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                9148
_reflns_number_total             9895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060937msup2.cif
_cod_data_source_block           4271a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      P2(1)2(1)2(1)
_cod_database_code               4332845