#------------------------------------------------------------------------------
#$Date: 2021-10-23 19:45:40 +0300 (Sat, 23 Oct 2021) $
#$Revision: 270066 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/00/4060017.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4060017
loop_
_publ_author_name
'Pillarsetty, Nagavarakishore'
'Raghuraman, Kannan'
'Barnes, Charles L.'
'Katti, Kattesh V.'
_publ_section_title
;
 Design, Synthesis, and Chemistry of Sterically Nondemanding Primary
 Bisphosphines¹
;
_journal_coden_ASTM              JACSAT
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              331
_journal_page_last               336
_journal_paper_doi               10.1021/ja047238y
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C10.17 H11 Cl0.25 N O P2'
_chemical_formula_weight         234.03
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   21.5254(13)
_cell_length_b                   21.5254(13)
_cell_length_c                   14.1730(12)
_cell_measurement_reflns_used    2391
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.6
_cell_volume                     5687.2(7)
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11927
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.8817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2183
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1084P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                1475
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4060017
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.05950(7) 0.24149(7) 0.25783(8) 0.0641(4) Uani 1 1 d . . .
H1P1 H 0.094(2) 0.305(2) 0.240(3) 0.071(12) Uiso 1 1 d . . .
H2P1 H 0.0605(18) 0.2456(17) 0.347(2) 0.057(10) Uiso 1 1 d . . .
P2 P -0.17372(8) 0.29951(9) 0.29827(10) 0.0894(5) Uani 1 1 d D . .
H1P2 H -0.1346(19) 0.3577(15) 0.254(3) 0.094(14) Uiso 1 1 d D . .
H2P2 H -0.169(3) 0.296(3) 0.3875(15) 0.15(2) Uiso 1 1 d D . .
O1 O -0.00761(12) 0.36367(11) 0.16274(14) 0.0402(6) Uani 1 1 d . . .
N1 N 0.03240(13) 0.39552(13) 0.31308(16) 0.0304(6) Uani 1 1 d . . .
H1 H 0.0251 0.3804 0.3719 0.036 Uiso 1 1 calc R . .
C1 C -0.00915(16) 0.34771(16) 0.2464(2) 0.0322(7) Uani 1 1 d . . .
C2 C -0.05700(17) 0.27136(16) 0.2805(2) 0.0364(8) Uani 1 1 d . . .
H2 H -0.0526 0.2699 0.3506 0.044 Uiso 1 1 calc R . .
C3 C -0.13540(19) 0.2454(2) 0.2551(2) 0.0491(9) Uani 1 1 d . . .
H3A H -0.1651 0.1961 0.2798 0.059 Uiso 1 1 calc R . .
H3B H -0.1397 0.2427 0.1855 0.059 Uiso 1 1 calc R . .
C4 C -0.0325(2) 0.22248(19) 0.2350(2) 0.0457(9) Uani 1 1 d . . .
H4A H -0.0383 0.2238 0.1659 0.055 Uiso 1 1 calc R . .
H4B H -0.0658 0.1728 0.2560 0.055 Uiso 1 1 calc R . .
C5 C 0.08628(16) 0.46740(16) 0.29736(19) 0.0286(7) Uani 1 1 d . . .
C6 C 0.14704(17) 0.49608(17) 0.3538(2) 0.0351(8) Uani 1 1 d . . .
H6 H 0.1511 0.4676 0.4019 0.042 Uiso 1 1 calc R . .
C7 C 0.20160(18) 0.56570(19) 0.3406(2) 0.0449(9) Uani 1 1 d . . .
H7 H 0.2428 0.5848 0.3799 0.054 Uiso 1 1 calc R . .
C8 C 0.1971(2) 0.60785(19) 0.2710(2) 0.0483(9) Uani 1 1 d . . .
H8 H 0.2350 0.6556 0.2618 0.058 Uiso 1 1 calc R . .
C9 C 0.1367(2) 0.57972(18) 0.2149(2) 0.0482(9) Uani 1 1 d . . .
H9 H 0.1335 0.6086 0.1665 0.058 Uiso 1 1 calc R . .
C10 C 0.08059(18) 0.51026(16) 0.2275(2) 0.0379(8) Uani 1 1 d . . .
H10 H 0.0388 0.4920 0.1893 0.046 Uiso 1 1 calc R . .
Cl1S Cl 0.31324(18) 0.58788(16) 0.5304(2) 0.115(3) Uiso 0.17 1 d PR . .
C1S C 0.33333(18) 0.66667(16) 0.5713(2) 0.075(4) Uiso 0.50 3 d SPR . .
Cl2S Cl 0.33333(18) 0.66667(16) 0.6262(2) 0.111(3) Uiso 0.25 3 d SPR . .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-23T19:30:00+03:00
'Updated bibliographic information.'
