#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:55:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179161 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312248.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_4312248
loop_
_publ_author_name
'Stuart Blair'
'Keith Izod'
'William Clegg'
'Ross W. Harrington'
_publ_section_title
;
 Complexes of the Heavier Alkaline Earth Metals Ca, Sr, and Ba with
 O-Functionalized Phosphanide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8526
_journal_page_last               8531
_journal_paper_doi               10.1021/ic048978a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C38 H72 Ba O4 P2 Si4'
_chemical_formula_weight         904.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.935(2)
_cell_angle_beta                 100.147(2)
_cell_angle_gamma                111.752(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4765(6)
_cell_length_b                   11.7093(8)
_cell_length_c                   12.9960(8)
_cell_measurement_reflns_used    8684
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.237
_cell_measurement_theta_min      2.375
_cell_volume                     1203.59(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'fine-slice ω 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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10075
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+0.1360P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                4800
_reflns_number_total             5316
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic048978asi20040728_063537_4.cif
_cod_data_source_block           8
_cod_original_cell_volume        1203.59(13)
_cod_database_code               4312248
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ba Ba 0.5000 0.5000 0.5000 0.03427(7) Uani 1 2 d S . .
P P 0.87501(6) 0.68437(5) 0.66067(4) 0.02921(11) Uani 1 1 d . . .
C1 C 0.8365(2) 0.57222(19) 0.73389(16) 0.0295(4) Uani 1 1 d . . .
C2 C 0.8864(3) 0.6112(2) 0.85343(18) 0.0373(5) Uani 1 1 d . . .
H2 H 0.9478 0.7041 0.9026 0.045 Uiso 1 1 calc R . .
C3 C 0.8482(3) 0.5175(3) 0.9011(2) 0.0473(6) Uani 1 1 d . . .
H3 H 0.8836 0.5473 0.9820 0.057 Uiso 1 1 calc R . .
C4 C 0.7592(3) 0.3813(3) 0.8325(2) 0.0519(6) Uani 1 1 d . . .
H4 H 0.7337 0.3184 0.8666 0.062 Uiso 1 1 calc R . .
C5 C 0.7067(3) 0.3357(2) 0.7139(2) 0.0434(5) Uani 1 1 d . . .
C6 C 0.7474(2) 0.4316(2) 0.66825(18) 0.0326(4) Uani 1 1 d . . .
O1 O 0.69003(16) 0.38541(14) 0.54813(12) 0.0354(3) Uani 1 1 d . . .
C7 C 0.8004(3) 0.3563(3) 0.4942(2) 0.0516(6) Uani 1 1 d . . .
H7A H 0.9039 0.4373 0.5252 0.077 Uiso 1 1 calc R . .
H7B H 0.7564 0.3279 0.4114 0.077 Uiso 1 1 calc R . .
H7C H 0.8158 0.2840 0.5092 0.077 Uiso 1 1 calc R . .
C8 C 0.6066(3) 0.1879(2) 0.6363(3) 0.0599(7) Uani 1 1 d . . .
H8A H 0.5058 0.1741 0.5867 0.090 Uiso 1 1 calc R . .
H8B H 0.5828 0.1359 0.6829 0.090 Uiso 1 1 calc R . .
H8C H 0.6665 0.1577 0.5891 0.090 Uiso 1 1 calc R . .
C9 C 0.9565(2) 0.85729(18) 0.77896(16) 0.0280(4) Uani 1 1 d . . .
H9 H 0.9227 0.8439 0.8448 0.034 Uiso 1 1 calc R . .
Si1 Si 0.84704(7) 0.94328(6) 0.72551(5) 0.03774(14) Uani 1 1 d . . .
C10 C 0.9312(4) 1.1240(3) 0.8274(3) 0.0807(11) Uani 1 1 d . . .
H10A H 0.8635 1.1630 0.8023 0.121 Uiso 1 1 calc R . .
H10B H 1.0408 1.1743 0.8286 0.121 Uiso 1 1 calc R . .
H10C H 0.9333 1.1292 0.9044 0.121 Uiso 1 1 calc R . .
C11 C 0.8545(4) 0.9385(4) 0.5819(3) 0.0676(8) Uani 1 1 d . . .
H11A H 0.8067 0.8447 0.5265 0.101 Uiso 1 1 calc R . .
H11B H 0.9666 0.9854 0.5863 0.101 Uiso 1 1 calc R . .
H11C H 0.7940 0.9830 0.5574 0.101 Uiso 1 1 calc R . .
C12 C 0.6302(3) 0.8597(3) 0.7138(2) 0.0532(6) Uani 1 1 d . . .
H12A H 0.6087 0.7802 0.7309 0.080 Uiso 1 1 calc R . .
H12B H 0.5621 0.8321 0.6359 0.080 Uiso 1 1 calc R . .
H12C H 0.6064 0.9229 0.7685 0.080 Uiso 1 1 calc R . .
Si2 Si 1.18186(7) 0.94535(6) 0.83098(5) 0.03590(13) Uani 1 1 d . . .
C13 C 1.2661(3) 1.1038(3) 0.9647(2) 0.0648(8) Uani 1 1 d . . .
H13A H 1.2146 1.0848 1.0207 0.097 Uiso 1 1 calc R . .
H13B H 1.2453 1.1723 0.9462 0.097 Uiso 1 1 calc R . .
H13C H 1.3824 1.1370 0.9970 0.097 Uiso 1 1 calc R . .
C14 C 1.2592(4) 0.9915(3) 0.7196(3) 0.0653(8) Uani 1 1 d . . .
H14A H 1.3752 1.0195 0.7412 0.098 Uiso 1 1 calc R . .
H14B H 1.2390 1.0657 0.7134 0.098 Uiso 1 1 calc R . .
H14C H 1.2041 0.9134 0.6456 0.098 Uiso 1 1 calc R . .
C15 C 1.2691(3) 0.8380(3) 0.8672(2) 0.0542(6) Uani 1 1 d . . .
H15A H 1.2500 0.8287 0.9366 0.081 Uiso 1 1 calc R . .
H15B H 1.3851 0.8800 0.8805 0.081 Uiso 1 1 calc R . .
H15C H 1.2179 0.7488 0.8037 0.081 Uiso 1 1 calc R . .
O2 O 0.3741(2) 0.4779(2) 0.67179(14) 0.0573(5) Uani 1 1 d U . .
C16 C 0.4603(4) 0.5293(4) 0.7902(2) 0.0798(10) Uani 1 1 d U A .
H16A H 0.5430 0.6236 0.8173 0.096 Uiso 0.490(12) 1 calc PR A 1
H16B H 0.5145 0.4749 0.8035 0.096 Uiso 0.490(12) 1 calc PR A 1
H16C H 0.4954 0.6273 0.8277 0.096 Uiso 0.510(12) 1 calc PR A 2
H16D H 0.5562 0.5132 0.8011 0.096 Uiso 0.510(12) 1 calc PR A 2
C17X C 0.3443(13) 0.5227(10) 0.8516(8) 0.065(2) Uani 0.490(12) 1 d PU A 1
H17A H 0.3683 0.6141 0.9043 0.078 Uiso 0.490(12) 1 calc PR A 1
H17B H 0.3468 0.4684 0.8965 0.078 Uiso 0.490(12) 1 calc PR A 1
C18X C 0.1808(11) 0.4563(9) 0.7592(8) 0.061(2) Uani 0.490(12) 1 d PU A 1
H18A H 0.0957 0.3961 0.7792 0.073 Uiso 0.490(12) 1 calc PR A 1
H18B H 0.1507 0.5242 0.7460 0.073 Uiso 0.490(12) 1 calc PR A 1
C19X C 0.2106(7) 0.3776(9) 0.6566(5) 0.0514(19) Uani 0.490(12) 1 d PU A 1
H19A H 0.2104 0.2941 0.6597 0.062 Uiso 0.490(12) 1 calc PR A 1
H19B H 0.1308 0.3548 0.5838 0.062 Uiso 0.490(12) 1 calc PR A 1
C17Y C 0.3474(16) 0.4563(19) 0.8370(12) 0.122(5) Uani 0.510(12) 1 d PU A 2
H17C H 0.3523 0.5186 0.9107 0.146 Uiso 0.510(12) 1 calc PR A 2
H17D H 0.3728 0.3862 0.8501 0.146 Uiso 0.510(12) 1 calc PR A 2
C18Y C 0.1811(12) 0.3924(14) 0.7486(10) 0.090(3) Uani 0.510(12) 1 d PU A 2
H18C H 0.1374 0.2932 0.7122 0.108 Uiso 0.510(12) 1 calc PR A 2
H18D H 0.1055 0.4149 0.7843 0.108 Uiso 0.510(12) 1 calc PR A 2
C19Y C 0.2074(7) 0.4509(10) 0.6636(5) 0.0534(19) Uani 0.510(12) 1 d PU A 2
H19C H 0.1320 0.3863 0.5857 0.064 Uiso 0.510(12) 1 calc PR A 2
H19D H 0.1957 0.5349 0.6841 0.064 Uiso 0.510(12) 1 calc PR A 2
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'
O O 0.0106 0.0060 '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'
Ba Ba -0.3244 2.2819 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P Ba P 180.0 . 2_666 ?
P Ba O1 59.08(3) . . ?
P Ba O1 59.08(3) 2_666 2_666 ?
P Ba O1 120.92(3) 2_666 . ?
P Ba O1 120.92(3) . 2_666 ?
P Ba O2 97.20(4) . . ?
P Ba O2 82.80(4) 2_666 . ?
P Ba O2 97.20(4) 2_666 2_666 ?
P Ba O2 82.80(4) . 2_666 ?
O1 Ba O1 180.0 . 2_666 ?
O1 Ba O2 93.30(5) . . ?
O1 Ba O2 86.70(5) 2_666 . ?
O1 Ba O2 93.30(5) 2_666 2_666 ?
O1 Ba O2 86.70(5) . 2_666 ?
O2 Ba O2 180.0 . 2_666 ?
Ba P C1 86.37(6) . . ?
Ba P C9 124.41(6) . . ?
C1 P C9 104.01(9) . . ?
P C1 C2 126.21(16) . . ?
P C1 C6 119.09(15) . . ?
C2 C1 C6 114.70(19) . . ?
C1 C2 C3 121.8(2) . . ?
C2 C3 C4 120.9(2) . . ?
C3 C4 C5 120.4(2) . . ?
C4 C5 C6 117.6(2) . . ?
C4 C5 C8 121.9(2) . . ?
C6 C5 C8 120.5(2) . . ?
C1 C6 C5 124.6(2) . . ?
C1 C6 O1 117.85(18) . . ?
C5 C6 O1 117.47(18) . . ?
Ba O1 C6 107.15(10) . . ?
Ba O1 C7 130.41(15) . . ?
C6 O1 C7 112.90(16) . . ?
P C9 Si1 106.26(9) . . ?
P C9 Si2 111.52(9) . . ?
Si1 C9 Si2 118.00(10) . . ?
C9 Si1 C10 111.35(11) . . ?
C9 Si1 C11 112.77(12) . . ?
C9 Si1 C12 109.94(11) . . ?
C10 Si1 C11 108.09(17) . . ?
C10 Si1 C12 106.74(15) . . ?
C11 Si1 C12 107.70(13) . . ?
C9 Si2 C13 112.25(11) . . ?
C9 Si2 C14 110.78(12) . . ?
C9 Si2 C15 111.87(10) . . ?
C13 Si2 C14 107.85(15) . . ?
C13 Si2 C15 106.00(13) . . ?
C14 Si2 C15 107.84(13) . . ?
Ba O2 C16 127.21(16) . . ?
Ba O2 C19X 126.0(2) . . ?
Ba O2 C19Y 123.8(3) . . ?
C16 O2 C19X 104.6(3) . . ?
C16 O2 C19Y 106.2(3) . . ?
O2 C16 C17X 107.5(4) . . ?
O2 C16 C17Y 105.1(6) . . ?
C16 C17X C18X 105.4(6) . . ?
C17X C18X C19X 101.8(7) . . ?
O2 C19X C18X 100.0(6) . . ?
C16 C17Y C18Y 106.3(8) . . ?
C17Y C18Y C19Y 104.5(8) . . ?
O2 C19Y C18Y 101.9(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba P 3.2516(5) . ?
Ba P 3.2516(5) 2_666 ?
Ba O1 2.7103(14) . ?
Ba O1 2.7103(14) 2_666 ?
Ba O2 2.7461(16) . ?
Ba O2 2.7461(17) 2_666 ?
P C1 1.817(2) . ?
P C9 1.8882(18) . ?
C1 C2 1.411(3) . ?
C1 C6 1.415(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.383(4) . ?
C4 C5 1.390(4) . ?
C5 C6 1.389(3) . ?
C5 C8 1.512(3) . ?
C6 O1 1.410(3) . ?
O1 C7 1.441(3) . ?
C9 Si1 1.877(2) . ?
C9 Si2 1.8741(19) . ?
Si1 C10 1.876(3) . ?
Si1 C11 1.865(3) . ?
Si1 C12 1.874(3) . ?
Si2 C13 1.878(2) . ?
Si2 C14 1.868(3) . ?
Si2 C15 1.867(3) . ?
O2 C16 1.421(3) . ?
O2 C19X 1.490(6) . ?
O2 C19Y 1.469(6) . ?
C16 C17X 1.461(11) . ?
C16 C17Y 1.455(13) . ?
C17X C18X 1.524(14) . ?
C18X C19X 1.509(11) . ?
C17Y C18Y 1.524(16) . ?
C18Y C19Y 1.479(15) . ?
