A Congestedin,in-Diphosphine
Zong, Jie; Mague, Joel T.; Kraml, Christina M.; Pascal, Robert A.; Organic Letters 15 (2013) 2179–; doi:10.1021/ol400728m

data_1511951
_publ_section_title
;
 A Congestedin,in-Diphosphine
;
_journal_issue                   9
_journal_name_full               'Organic Letters'
_journal_page_first              2179
_journal_paper_doi               10.1021/ol400728m
_journal_volume                  15
_journal_year                    2013
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C39 H31 Cl P2 S3, 2(C H Cl3), Cl, H2 O'
_chemical_formula_sum            'C41 H35 Cl7 O P2 S3'
_chemical_formula_weight         949.96
_chemical_name_common
;
 in,in-bis(triarylphosphine) hydrochloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.875(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.157(2)
_cell_length_b                   19.846(4)
_cell_length_c                   16.443(3)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.69
_cell_volume                     4278.0(13)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w 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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75153
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.8998
_exptl_absorpt_correction_T_min  0.7673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         11199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0406P)^2^+2.8727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                9721
_reflns_number_total             11199
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol400728m_si_002.cif
_cod_data_source_block           rap040_0m
_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_cell_volume        4277.9(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1511951