#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:44:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178665 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/76/4077614.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_4077614
loop_
_publ_author_name
'Tran, Diem T. T.'
'Corrigan, John F.'
_publ_section_title
;
 Synthesis and Characterization of
 Tris(trialkylphosphine)copper(I)trimethylsilylchalcogenolates
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5202
_journal_paper_doi               10.1021/om000624d
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C21 H54 Cu P3 S Si'
_chemical_formula_weight         523.24
_chemical_name_systematic
; 
 ? 
;
_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                 97.5700(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9276(4)
_cell_length_b                   13.9813(5)
_cell_length_c                   18.2051(5)
_cell_measurement_temperature    200(2)
_cell_volume                     3009.48(17)
_computing_cell_refinement       DenzoSMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DenzoSMN
_computing_molecular_graphics    'XP Version 5.10'
_computing_structure_refinement  'SHELXTL Version 5.10'
_computing_structure_solution    'SHELXTL Ver 5.10'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Phi frames plus omega to complete'
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17868
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0267
_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/[σ²(Fo²)+(0.0325P)²+0.3850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                4918
_reflns_number_total             5870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000624d.cif
_cod_data_source_block           for_compound_1a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077614
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu1 Cu 0.005721(17) 0.239573(14) 0.178365(11) 0.02443(7) Uani 1 1 d .
S1 S 0.16504(4) 0.33224(3) 0.15161(2) 0.03044(11) Uani 1 1 d .
Si1 Si 0.27120(5) 0.28132(4) 0.07840(3) 0.03557(14) Uani 1 1 d .
P1 P -0.12897(4) 0.24169(3) 0.07525(3) 0.02691(11) Uani 1 1 d .
P2 P 0.07249(4) 0.09207(3) 0.22007(2) 0.02672(11) Uani 1 1 d .
P3 P -0.04438(4) 0.33314(3) 0.27293(2) 0.02580(11) Uani 1 1 d .
C1 C -0.19135(16) 0.12649(14) 0.04350(10) 0.0381(5) Uani 1 1 d .
H1A H -0.2382 0.1360 -0.0037 0.046 Uiso 1 1 calc R
H1B H -0.1310 0.0829 0.0353 0.046 Uiso 1 1 calc R
C2 C -0.26250(18) 0.08045(16) 0.09720(12) 0.0519(6) Uani 1 1 d .
H2A H -0.2924 0.0208 0.0771 0.078 Uiso 1 1 calc R
H2B H -0.3237 0.1224 0.1048 0.078 Uiso 1 1 calc R
H2C H -0.2163 0.0690 0.1437 0.078 Uiso 1 1 calc R
C3 C -0.08096(16) 0.28264(15) -0.01074(10) 0.0380(5) Uani 1 1 d .
H3A H -0.0146 0.2461 -0.0189 0.046 Uiso 1 1 calc R
H3B H -0.1396 0.2692 -0.0516 0.046 Uiso 1 1 calc R
C4 C -0.0522(2) 0.38825(17) -0.01186(12) 0.0574(6) Uani 1 1 d .
H4A H -0.0278 0.4042 -0.0585 0.086 Uiso 1 1 calc R
H4B H 0.0073 0.4022 0.0275 0.086 Uiso 1 1 calc R
H4C H -0.1179 0.4253 -0.0053 0.086 Uiso 1 1 calc R
C5 C -0.25466(15) 0.31648(16) 0.07966(10) 0.0389(5) Uani 1 1 d .
H5A H -0.2914 0.2944 0.1210 0.047 Uiso 1 1 calc R
H5B H -0.2292 0.3814 0.0908 0.047 Uiso 1 1 calc R
C6 C -0.34407(17) 0.31975(18) 0.01068(11) 0.0504(6) Uani 1 1 d .
H6A H -0.4049 0.3611 0.0200 0.076 Uiso 1 1 calc R
H6B H -0.3728 0.2565 -0.0003 0.076 Uiso 1 1 calc R
H6C H -0.3103 0.3437 -0.0307 0.076 Uiso 1 1 calc R
C7 C 0.03735(17) -0.01013(14) 0.15676(11) 0.0425(5) Uani 1 1 d .
H7A H -0.0444 -0.0135 0.1460 0.051 Uiso 1 1 calc R
H7B H 0.0659 0.0044 0.1105 0.051 Uiso 1 1 calc R
C8 C 0.0797(2) -0.10848(16) 0.18113(14) 0.0589(6) Uani 1 1 d .
H8A H 0.0553 -0.1540 0.1429 0.088 Uiso 1 1 calc R
H8B H 0.0498 -0.1260 0.2257 0.088 Uiso 1 1 calc R
H8C H 0.1608 -0.1079 0.1903 0.088 Uiso 1 1 calc R
C9 C 0.22683(14) 0.08545(13) 0.23746(10) 0.0325(4) Uani 1 1 d .
H9A H 0.2491 0.0207 0.2520 0.039 Uiso 1 1 calc R
H9B H 0.2576 0.0998 0.1920 0.039 Uiso 1 1 calc R
C10 C 0.27698(15) 0.15471(15) 0.29793(11) 0.0406(5) Uani 1 1 d .
H10A H 0.3579 0.1487 0.3051 0.061 Uiso 1 1 calc R
H10B H 0.2480 0.1399 0.3434 0.061 Uiso 1 1 calc R
H10C H 0.2565 0.2190 0.2833 0.061 Uiso 1 1 calc R
C11 C 0.03781(15) 0.04718(14) 0.30923(10) 0.0364(4) Uani 1 1 d .
H11A H 0.0853 -0.0078 0.3238 0.044 Uiso 1 1 calc R
H11B H 0.0559 0.0964 0.3465 0.044 Uiso 1 1 calc R
C12 C -0.08617(17) 0.01811(16) 0.30846(12) 0.0503(6) Uani 1 1 d .
H12A H -0.0977 -0.0046 0.3567 0.075 Uiso 1 1 calc R
H12B H -0.1046 -0.0318 0.2727 0.075 Uiso 1 1 calc R
H12C H -0.1339 0.0724 0.2955 0.075 Uiso 1 1 calc R
C13 C 0.07899(15) 0.37364(14) 0.33623(10) 0.0358(4) Uani 1 1 d .
H13A H 0.1132 0.3179 0.3618 0.043 Uiso 1 1 calc R
H13B H 0.1336 0.3992 0.3064 0.043 Uiso 1 1 calc R
C14 C 0.06089(18) 0.44835(16) 0.39465(12) 0.0531(6) Uani 1 1 d .
H14A H 0.1320 0.4630 0.4236 0.080 Uiso 1 1 calc R
H14B H 0.0096 0.4236 0.4264 0.080 Uiso 1 1 calc R
H14C H 0.0297 0.5054 0.3707 0.080 Uiso 1 1 calc R
C15 C -0.11758(14) 0.44547(13) 0.24545(10) 0.0325(4) Uani 1 1 d .
H15A H -0.1899 0.4308 0.2167 0.039 Uiso 1 1 calc R
H15B H -0.1325 0.4793 0.2897 0.039 Uiso 1 1 calc R
C16 C -0.05133(18) 0.51040(15) 0.20031(13) 0.0502(6) Uani 1 1 d .
H16A H -0.0938 0.5678 0.1878 0.075 Uiso 1 1 calc R
H16B H -0.0379 0.4781 0.1557 0.075 Uiso 1 1 calc R
H16C H 0.0197 0.5264 0.2288 0.075 Uiso 1 1 calc R
C17 C -0.13570(17) 0.28465(15) 0.33773(11) 0.0415(5) Uani 1 1 d .
H17A H -0.0998 0.2284 0.3616 0.050 Uiso 1 1 calc R
H17B H -0.1425 0.3318 0.3760 0.050 Uiso 1 1 calc R
C18 C -0.25401(18) 0.25755(16) 0.30101(14) 0.0561(6) Uani 1 1 d .
H18A H -0.2971 0.2327 0.3377 0.084 Uiso 1 1 calc R
H18B H -0.2482 0.2097 0.2639 0.084 Uiso 1 1 calc R
H18C H -0.2910 0.3132 0.2784 0.084 Uiso 1 1 calc R
C19 C 0.2925(2) 0.37575(17) 0.00798(12) 0.0594(6) Uani 1 1 d .
H19A H 0.3416 0.3516 -0.0255 0.089 Uiso 1 1 calc R
H19B H 0.3260 0.4314 0.0328 0.089 Uiso 1 1 calc R
H19C H 0.2208 0.3925 -0.0193 0.089 Uiso 1 1 calc R
C20 C 0.21969(18) 0.17078(15) 0.02538(12) 0.0500(6) Uani 1 1 d .
H20A H 0.2735 0.1524 -0.0068 0.075 Uiso 1 1 calc R
H20B H 0.1481 0.1838 -0.0036 0.075 Uiso 1 1 calc R
H20C H 0.2112 0.1198 0.0595 0.075 Uiso 1 1 calc R
C21 C 0.41671(17) 0.25086(16) 0.12613(13) 0.0511(6) Uani 1 1 d .
H21A H 0.4624 0.2278 0.0903 0.077 Uiso 1 1 calc R
H21B H 0.4109 0.2023 0.1627 0.077 Uiso 1 1 calc R
H21C H 0.4510 0.3070 0.1497 0.077 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P3 Cu1 P2 112.009(18)
P3 Cu1 P1 112.329(18)
P2 Cu1 P1 116.981(18)
P3 Cu1 S1 97.774(17)
P2 Cu1 S1 107.541(18)
P1 Cu1 S1 108.245(18)
Si1 S1 Cu1 120.64(3)
C19 Si1 C20 106.93(11)
C19 Si1 C21 105.91(11)
C20 Si1 C21 105.64(10)
C19 Si1 S1 110.16(7)
C20 Si1 S1 115.11(7)
C21 Si1 S1 112.52(8)
C3 P1 C1 99.48(9)
C3 P1 C5 102.04(9)
C1 P1 C5 102.35(9)
C3 P1 Cu1 115.98(6)
C1 P1 Cu1 117.09(6)
C5 P1 Cu1 117.18(6)
C9 P2 C11 99.69(9)
C9 P2 C7 102.07(9)
C11 P2 C7 103.16(10)
C9 P2 Cu1 113.51(6)
C11 P2 Cu1 119.26(7)
C7 P2 Cu1 116.52(7)
C15 P3 C13 102.75(9)
C15 P3 C17 100.94(9)
C13 P3 C17 101.82(9)
C15 P3 Cu1 116.33(6)
C13 P3 Cu1 112.28(6)
C17 P3 Cu1 120.30(7)
C2 C1 P1 114.00(15)
C4 C3 P1 114.41(15)
C6 C5 P1 117.60(14)
C8 C7 P2 118.74(15)
C10 C9 P2 112.47(12)
C12 C11 P2 114.32(13)
C14 C13 P3 118.26(13)
C16 C15 P3 113.42(13)
C18 C17 P3 113.72(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu1 P3 2.3029(5)
Cu1 P2 2.3031(5)
Cu1 P1 2.3046(5)
Cu1 S1 2.4022(5)
S1 Si1 2.0812(6)
Si1 C19 1.881(2)
Si1 C20 1.882(2)
Si1 C21 1.884(2)
P1 C3 1.8283(18)
P1 C1 1.8354(19)
P1 C5 1.8381(19)
P2 C9 1.8288(17)
P2 C11 1.8377(18)
P2 C7 1.8489(19)
P3 C15 1.8342(18)
P3 C13 1.8350(18)
P3 C17 1.8375(18)
C1 C2 1.520(3)
C3 C4 1.517(3)
C5 C6 1.537(3)
C7 C8 1.511(3)
C9 C10 1.528(3)
C11 C12 1.532(3)
C13 C14 1.526(3)
C15 C16 1.515(3)
C17 C18 1.527(3)
