Chiral Birch reduced tertiary phosphines: precursors to asymmetric 1,2-cyclohexenebis(tertiary phosphines).
Bulbrook, Michelle; Chu, Minghui; Deane, Karen; Doyle, Roy J.; Hinc, Justina; Peterson, Charlotte; Salem, Geoffrey; Thorman, Nadia; Willis, Anthony C.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 8878–8881; doi:10.1039/c0dt00648c

data_7026741
_publ_section_title
;
 Chiral Birch reduced tertiary phosphines: precursors to asymmetric
 1,2-cyclohexenebis(tertiary phosphines).
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8878
_journal_page_last               8881
_journal_paper_doi               10.1039/c0dt00648c
_journal_volume                  39
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        local
_chemical_formula_moiety         ' C27 H37 Cl N P Pd, 0.5(C4 H8 O)'
_chemical_formula_sum            'C29 H41 Cl N O0.5 P Pd'
_chemical_formula_weight         584.48
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-10-22
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2008-10-22 - Report on 'C29 H41 Cl N O0.5 P Pd
by Anthony C. Willis
for Geoff Salem and Minghui Chu

2008-10-22 - passes checkcif tests with minor warnings
2008-10-23 - fix up error
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.5899(2)
_cell_length_b                   11.5899(2)
_cell_length_c                   42.4182(8)
_cell_measurement_reflns_used    101202
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     5697.86(18)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_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      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            51750
_diffrn_reflns_theta_full        27.439
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_min         2.664
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995,1997)
implemented in maxus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.69
_refine_ls_abs_structure_details 'Flack (1983), 2674 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8527
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6487
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.047563
_refine_ls_structure_factor_coef Fsqd
_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:
13.8 20.4 10.8 3.28
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0879
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0879
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              54
_reflns_limit_l_min              0
_reflns_number_gt                4703
_reflns_number_total             6487
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.30
_oxford_diffrn_Wilson_scale      55.89
_oxford_refine_ls_r_factor_ref   0.0446
_oxford_refine_ls_scale          0.14540(5)
_oxford_reflns_number_all        6487
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '10211636 sal0801'
_cod_data_source_file            c0dt00648c.txt
_cod_data_source_block           sal0801a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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      'P 43 21 2 '
_cod_original_formula_sum        'C29 H41 Cl N O0.50 P Pd'
_cod_database_code               7026741