#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:55:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179161 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312249.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_4312249
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_moiety         'C38 H72 Ca O4 P2 Si4'
_chemical_formula_sum            'C38 H72 Ca O4 P2 Si4'
_chemical_formula_weight         807.34
_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                 118.796(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.259(8)
_cell_length_b                   17.560(10)
_cell_length_c                   12.588(14)
_cell_measurement_reflns_used    17158
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      1.91
_cell_volume                     2375(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4611
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0905P)²+3.1797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                3827
_reflns_number_total             4613
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic048978asi20040728_063537_5.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4312249
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca Ca 0.5000 0.5000 0.5000 0.0209(3) Uani 1 2 d S . .
P P 0.44865(10) 0.59164(6) 0.66217(9) 0.0242(3) Uani 1 1 d . . .
Si1 Si 0.31064(12) 0.68317(7) 0.76547(11) 0.0291(3) Uani 1 1 d . . .
Si2 Si 0.29702(12) 0.49862(7) 0.75357(12) 0.0336(3) Uani 1 1 d . . .
O1 O 0.6217(3) 0.61402(17) 0.5646(3) 0.0285(7) Uani 1 1 d . . .
O2 O 0.3259(3) 0.56148(19) 0.3330(3) 0.0366(8) Uani 1 1 d DU . .
C1 C 0.3883(4) 0.5885(2) 0.7742(4) 0.0251(9) Uani 1 1 d . . .
H1 H 0.4628 0.5856 0.8567 0.030 Uiso 1 1 calc R . .
C2 C 0.4125(5) 0.7649(3) 0.7771(4) 0.0387(11) Uani 1 1 d . . .
H2C H 0.4386 0.7599 0.7151 0.046 Uiso 1 1 calc R . .
H2B H 0.4861 0.7651 0.8576 0.046 Uiso 1 1 calc R . .
H2A H 0.3665 0.8126 0.7648 0.046 Uiso 1 1 calc R . .
C3 C 0.2759(6) 0.6967(3) 0.8955(5) 0.0508(14) Uani 1 1 d . . .
H3C H 0.3526 0.6903 0.9727 0.061 Uiso 1 1 calc R . .
H3B H 0.2144 0.6589 0.8896 0.061 Uiso 1 1 calc R . .
H3A H 0.2427 0.7480 0.8917 0.061 Uiso 1 1 calc R . .
C4 C 0.1618(5) 0.6897(3) 0.6181(4) 0.0443(12) Uani 1 1 d . . .
H4C H 0.1243 0.7400 0.6112 0.053 Uiso 1 1 calc R . .
H4B H 0.1040 0.6503 0.6154 0.053 Uiso 1 1 calc R . .
H4A H 0.1794 0.6822 0.5506 0.053 Uiso 1 1 calc R . .
C5 C 0.2057(6) 0.5013(4) 0.8375(6) 0.0643(18) Uani 1 1 d . . .
H5C H 0.1535 0.4556 0.8179 0.077 Uiso 1 1 calc R . .
H5B H 0.1528 0.5467 0.8135 0.077 Uiso 1 1 calc R . .
H5A H 0.2630 0.5028 0.9249 0.077 Uiso 1 1 calc R . .
C6 C 0.4086(6) 0.4166(3) 0.8200(6) 0.0541(15) Uani 1 1 d . . .
H6A H 0.4559 0.4105 0.7761 0.065 Uiso 1 1 calc R . .
H6B H 0.3620 0.3698 0.8127 0.065 Uiso 1 1 calc R . .
H6C H 0.4662 0.4267 0.9057 0.065 Uiso 1 1 calc R . .
C7 C 0.1857(5) 0.4775(4) 0.5897(5) 0.0545(15) Uani 1 1 d . . .
H7A H 0.2319 0.4737 0.5444 0.065 Uiso 1 1 calc R . .
H7B H 0.1242 0.5185 0.5556 0.065 Uiso 1 1 calc R . .
H7C H 0.1430 0.4292 0.5837 0.065 Uiso 1 1 calc R . .
C8 C 0.6088(4) 0.6226(2) 0.7499(4) 0.0271(9) Uani 1 1 d . . .
C9 C 0.6723(4) 0.6411(3) 0.8753(4) 0.0334(10) Uani 1 1 d . . .
H9 H 0.6282 0.6407 0.9200 0.040 Uiso 1 1 calc R . .
C10 C 0.7969(5) 0.6595(3) 0.9330(4) 0.0428(12) Uani 1 1 d . . .
H10 H 0.8370 0.6703 1.0174 0.051 Uiso 1 1 calc R . .
C11 C 0.8656(4) 0.6626(3) 0.8722(4) 0.0373(11) Uani 1 1 d . . .
H11 H 0.9518 0.6745 0.9148 0.045 Uiso 1 1 calc R . .
C12 C 0.8066(4) 0.6481(3) 0.7464(4) 0.0327(10) Uani 1 1 d . . .
C13 C 0.6814(4) 0.6293(2) 0.6905(4) 0.0250(9) Uani 1 1 d . . .
C14 C 0.5668(5) 0.6820(3) 0.4936(4) 0.0416(12) Uani 1 1 d . . .
H14C H 0.5042 0.7024 0.5131 0.050 Uiso 1 1 calc R . .
H14B H 0.5273 0.6693 0.4071 0.050 Uiso 1 1 calc R . .
H14A H 0.6319 0.7202 0.5124 0.050 Uiso 1 1 calc R . .
C15 C 0.8793(4) 0.6520(3) 0.6787(5) 0.0431(12) Uani 1 1 d . . .
H15A H 0.8416 0.6178 0.6085 0.065 Uiso 1 1 calc R . .
H15B H 0.9655 0.6363 0.7323 0.065 Uiso 1 1 calc R . .
H15C H 0.8783 0.7043 0.6511 0.065 Uiso 1 1 calc R . .
C16 C 0.2293(16) 0.6103(11) 0.3344(15) 0.046(5) Uani 0.473(15) 1 d PDU A 1
H16B H 0.1742 0.5790 0.3541 0.056 Uiso 0.473(15) 1 calc PR A 1
H16A H 0.2692 0.6493 0.3987 0.056 Uiso 0.473(15) 1 calc PR A 1
C16A C 0.2119(13) 0.5855(11) 0.3325(14) 0.049(5) Uani 0.527(15) 1 d PDU A 2
H16D H 0.2270 0.6319 0.3823 0.059 Uiso 0.527(15) 1 calc PR A 2
H16C H 0.1812 0.5448 0.3658 0.059 Uiso 0.527(15) 1 calc PR A 2
C17 C 0.1593(16) 0.6458(9) 0.2253(13) 0.056(4) Uani 0.473(15) 1 d PDU A 1
H17B H 0.1617 0.7018 0.2353 0.067 Uiso 0.473(15) 1 calc PR A 1
H17A H 0.0717 0.6285 0.1869 0.067 Uiso 0.473(15) 1 calc PR A 1
C17A C 0.1269(14) 0.5999(13) 0.2137(12) 0.081(5) Uani 0.527(15) 1 d PDU A 2
H17D H 0.1167 0.6556 0.2002 0.097 Uiso 0.527(15) 1 calc PR A 2
H17C H 0.0451 0.5781 0.1952 0.097 Uiso 0.527(15) 1 calc PR A 2
C18 C 0.2197(14) 0.6224(9) 0.1519(11) 0.055(4) Uani 0.473(15) 1 d PDU A 1
H18B H 0.1580 0.5962 0.0773 0.066 Uiso 0.473(15) 1 calc PR A 1
H18A H 0.2494 0.6682 0.1275 0.066 Uiso 0.473(15) 1 calc PR A 1
C18A C 0.1696(10) 0.5659(9) 0.1322(9) 0.056(4) Uani 0.527(15) 1 d PDU A 2
H18C H 0.1208 0.5198 0.0914 0.068 Uiso 0.527(15) 1 calc PR A 2
H18D H 0.1630 0.6028 0.0700 0.068 Uiso 0.527(15) 1 calc PR A 2
C19 C 0.3131(16) 0.5770(11) 0.2141(12) 0.050(5) Uani 0.473(15) 1 d PDU A 1
H19B H 0.3907 0.6006 0.2237 0.060 Uiso 0.473(15) 1 calc PR A 1
H19A H 0.3003 0.5285 0.1695 0.060 Uiso 0.473(15) 1 calc PR A 1
C19A C 0.2838(13) 0.5491(9) 0.2050(8) 0.046(4) Uani 0.527(15) 1 d PDU A 2
H19D H 0.3371 0.5794 0.1819 0.055 Uiso 0.527(15) 1 calc PR A 2
H19C H 0.2968 0.4947 0.1933 0.055 Uiso 0.527(15) 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'
Ca Ca 0.2262 0.3064 '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 Ca P 180.00(3) . 3_666 ?
P Ca O1 66.86(8) . . ?
P Ca O1 113.14(8) . 3_666 ?
P Ca O1 66.86(8) 3_666 3_666 ?
P Ca O1 113.14(8) 3_666 . ?
P Ca O2 87.95(10) . . ?
P Ca O2 92.05(10) . 3_666 ?
P Ca O2 92.05(10) 3_666 . ?
P Ca O2 87.95(10) 3_666 3_666 ?
O1 Ca O1 180.0 . 3_666 ?
O1 Ca O2 93.83(12) . . ?
O1 Ca O2 86.17(12) 3_666 . ?
O1 Ca O2 93.82(12) 3_666 3_666 ?
O1 Ca O2 86.18(12) . 3_666 ?
O2 Ca O2 179.998(1) . 3_666 ?
Ca P C1 143.98(14) . . ?
Ca P C8 93.26(14) . . ?
C1 P C8 104.7(2) . . ?
C1 Si1 C2 111.9(2) . . ?
C1 Si1 C3 112.1(2) . . ?
C1 Si1 C4 109.5(2) . . ?
C2 Si1 C3 104.9(2) . . ?
C2 Si1 C4 109.1(2) . . ?
C3 Si1 C4 109.3(3) . . ?
C1 Si2 C5 112.3(2) . . ?
C1 Si2 C6 108.9(2) . . ?
C1 Si2 C7 112.7(2) . . ?
C5 Si2 C6 105.8(3) . . ?
C5 Si2 C7 108.0(3) . . ?
C6 Si2 C7 108.9(3) . . ?
Ca O1 C13 116.1(2) . . ?
Ca O1 C14 116.8(3) . . ?
C13 O1 C14 111.8(3) . . ?
Ca O2 C16 129.1(7) . . ?
Ca O2 C16A 125.3(6) . . ?
Ca O2 C19 126.4(6) . . ?
Ca O2 C19A 126.3(5) . . ?
C16 O2 C19 102.4(9) . . ?
C16A O2 C19A 102.2(9) . . ?
P C1 Si1 107.4(2) . . ?
P C1 Si2 110.1(2) . . ?
Si1 C1 Si2 118.7(2) . . ?
P C8 C9 126.8(3) . . ?
P C8 C13 118.4(3) . . ?
C9 C8 C13 114.9(4) . . ?
C8 C9 C10 121.0(4) . . ?
C9 C10 C11 122.2(4) . . ?
C10 C11 C12 119.5(4) . . ?
C11 C12 C13 117.2(4) . . ?
C11 C12 C15 120.3(4) . . ?
C13 C12 C15 122.5(4) . . ?
O1 C13 C8 117.3(4) . . ?
O1 C13 C12 117.6(4) . . ?
C8 C13 C12 125.1(4) . . ?
O2 C16 C17 111.9(11) . . ?
O2 C16A C17A 106.3(11) . . ?
C16 C17 C18 103.7(10) . . ?
C16A C17A C18A 110.1(11) . . ?
C17 C18 C19 110.5(10) . . ?
C17A C18A C19A 103.0(10) . . ?
O2 C19 C18 111.2(11) . . ?
O2 C19A C18A 116.1(10) . . ?
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
Ca P 2.897(2) . ?
Ca P 2.897(2) 3_666 ?
Ca O1 2.393(3) . ?
Ca O1 2.393(3) 3_666 ?
Ca O2 2.412(3) . ?
Ca O2 2.412(3) 3_666 ?
P C1 1.883(4) . ?
P C8 1.812(5) . ?
Si1 C1 1.893(4) . ?
Si1 C2 1.861(5) . ?
Si1 C3 1.895(5) . ?
Si1 C4 1.877(5) . ?
Si2 C1 1.879(4) . ?
Si2 C5 1.874(5) . ?
Si2 C6 1.883(6) . ?
Si2 C7 1.883(6) . ?
O1 C13 1.415(5) . ?
O1 C14 1.448(6) . ?
O2 C16 1.469(12) . ?
O2 C16A 1.457(11) . ?
O2 C19 1.453(12) . ?
O2 C19A 1.452(10) . ?
C8 C9 1.421(6) . ?
C8 C13 1.416(6) . ?
C9 C10 1.377(7) . ?
C10 C11 1.386(7) . ?
C11 C12 1.410(6) . ?
C12 C13 1.386(6) . ?
C12 C15 1.503(6) . ?
C16 C17 1.370(13) . ?
C16A C17A 1.374(13) . ?
C17 C18 1.493(13) . ?
C17A C18A 1.484(13) . ?
C18 C19 1.302(13) . ?
C18A C19A 1.285(12) . ?
