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_7026742
_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_compound_source        local
_chemical_formula_moiety         'C29 H36 P2 Pt'
_chemical_formula_sum            'C29 H36 P2 Pt'
_chemical_formula_weight         641.64
_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             10-05-18
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-05-18 - Report on C29 H36 P2 Pt
by Anthony C. Willis
for Geoff Salem and Roy Doylen

2010-05-18 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5919(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2514(1)
_cell_length_b                   16.8489(2)
_cell_length_c                   15.6183(2)
_cell_measurement_reflns_used    71654
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.6
_cell_volume                     2674.02(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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  0.052
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69946
_diffrn_reflns_theta_full        30.086
_diffrn_reflns_theta_max         30.086
_diffrn_reflns_theta_min         2.552
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.382
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272.000
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         4.26
_refine_diff_density_min         -1.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7847
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.0242266
_refine_ls_shift/su_mean         0.0066263
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 8.39P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0874
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0874
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6546
_reflns_number_total             7853
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.80
_oxford_diffrn_Wilson_scale      18.60
_oxford_refine_ls_r_factor_ref   0.0453
_oxford_refine_ls_scale          0.3397(2)
_oxford_reflns_number_all        7847
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '4121217 sal1001'
_cod_data_source_file            c0dt00648c.txt
_cod_data_source_block           sal1001
_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 2.4.2 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 1 21/c 1 '
_cod_database_code               7026742