#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/92/4319291.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_4319291
loop_
_publ_author_name
'Maarten B. Dinger'
'Michael J. Scott'
_publ_contact_author_address
;
P.O. Box 117200
University of Florida
Gainesville FL, 32611
;
_publ_contact_author_name        'Maarten B. Dinger and Michael J. Scott'
_publ_section_title
;
 Sterically Crowded, Rigid,C3 Symmetric Phosphites: Synthesis, Structure,
 and Preparation of Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              856
_journal_page_last               864
_journal_paper_doi               10.1021/ic000683j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C46 H55 As O3'
_chemical_formula_weight         730.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.4932(14)
_cell_length_b                   26.4932(14)
_cell_length_c                   27.759(2)
_cell_measurement_temperature    173(2)
_cell_volume                     16873.4(18)
_computing_cell_refinement       'Bruker AXS SMART'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1123
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38882
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.874862
_exptl_absorpt_correction_T_min  0.641992
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6984
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0449
_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)+(0.0687P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                7176
_reflns_number_total             9227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000683j_2.cif
_cod_data_source_block           3b
_cod_original_cell_volume        16873.6(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4319291
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
As1 As 0.752618(8) 0.658847(9) 0.165019(7) 0.03296(8) Uani 1 1 d . . .
O1 O 0.71198(5) 0.64406(6) 0.21920(4) 0.0318(3) Uani 1 1 d . . .
C1 C 0.62576(8) 0.65692(8) 0.16147(6) 0.0287(4) Uani 1 1 d . . .
H1A H 0.5880 0.6569 0.1602 0.034 Uiso 1 1 calc R . .
O2 O 0.75243(6) 0.72282(6) 0.14513(5) 0.0338(3) Uani 1 1 d . . .
C2 C 0.61210(8) 0.60675(8) 0.19602(6) 0.0277(4) Uani 1 1 d . . .
O3 O 0.69670(6) 0.60593(6) 0.12797(4) 0.0328(3) Uani 1 1 d . . .
C3 C 0.65332(8) 0.60149(8) 0.22309(6) 0.0289(4) Uani 1 1 d . . .
C4 C 0.63766(8) 0.55474(8) 0.25536(6) 0.0312(4) Uani 1 1 d . . .
C5 C 0.68315(9) 0.54637(9) 0.28327(7) 0.0371(4) Uani 1 1 d . . .
C6 C 0.65405(12) 0.49170(11) 0.31520(9) 0.0559(6) Uani 1 1 d . . .
H6A H 0.6287 0.4956 0.3388 0.084 Uiso 1 1 calc R . .
H6B H 0.6841 0.4873 0.3321 0.084 Uiso 1 1 calc R . .
H6C H 0.6308 0.4573 0.2951 0.084 Uiso 1 1 calc R . .
C7 C 0.71980(11) 0.59850(11) 0.31628(8) 0.0521(6) Uani 1 1 d . . .
H7A H 0.6941 0.6040 0.3384 0.078 Uiso 1 1 calc R . .
H7B H 0.7418 0.6337 0.2967 0.078 Uiso 1 1 calc R . .
H7C H 0.7469 0.5912 0.3349 0.078 Uiso 1 1 calc R . .
C8 C 0.72286(12) 0.53787(13) 0.24793(9) 0.0567(6) Uani 1 1 d . . .
H8A H 0.6989 0.5070 0.2249 0.085 Uiso 1 1 calc R . .
H8B H 0.7478 0.5269 0.2658 0.085 Uiso 1 1 calc R . .
H8C H 0.7472 0.5743 0.2305 0.085 Uiso 1 1 calc R . .
C9 C 0.57839(9) 0.51601(8) 0.26067(6) 0.0333(4) Uani 1 1 d . . .
H9A H 0.5665 0.4850 0.2830 0.040 Uiso 1 1 calc R . .
C10 C 0.53563(8) 0.52022(8) 0.23505(6) 0.0337(4) Uani 1 1 d . . .
C11 C 0.47177(9) 0.47848(9) 0.24388(7) 0.0420(5) Uani 1 1 d . . .
H11A H 0.4488 0.4813 0.2174 0.063 Uiso 1 1 calc R . .
H11B H 0.4600 0.4884 0.2743 0.063 Uiso 1 1 calc R . .
H11C H 0.4649 0.4386 0.2457 0.063 Uiso 1 1 calc R . .
C12 C 0.55326(8) 0.56531(8) 0.20247(6) 0.0309(4) Uani 1 1 d . . .
H12A H 0.5247 0.5683 0.1839 0.037 Uiso 1 1 calc R . .
C13 C 0.66777(8) 0.71723(8) 0.18170(6) 0.0299(4) Uani 1 1 d . . .
C14 C 0.72693(8) 0.74886(8) 0.17157(6) 0.0317(4) Uani 1 1 d . . .
C15 C 0.76223(9) 0.80750(9) 0.18652(7) 0.0352(4) Uani 1 1 d . . .
C16 C 0.82697(9) 0.84387(10) 0.17214(8) 0.0442(5) Uani 1 1 d . . .
C17 C 0.83315(11) 0.84631(11) 0.11690(8) 0.0513(6) Uani 1 1 d . . .
H17A H 0.8105 0.8628 0.1031 0.077 Uiso 1 1 calc R . .
H17B H 0.8186 0.8069 0.1043 0.077 Uiso 1 1 calc R . .
H17C H 0.8743 0.8709 0.1082 0.077 Uiso 1 1 calc R . .
C18 C 0.85377(13) 0.90772(12) 0.18972(12) 0.0716(8) Uani 1 1 d . . .
H18A H 0.8317 0.9250 0.1761 0.107 Uiso 1 1 calc R . .
H18B H 0.8945 0.9302 0.1792 0.107 Uiso 1 1 calc R . .
H18C H 0.8520 0.9084 0.2250 0.107 Uiso 1 1 calc R . .
C19 C 0.86244(11) 0.81853(13) 0.19456(10) 0.0604(7) Uani 1 1 d . . .
H19A H 0.9039 0.8442 0.1874 0.091 Uiso 1 1 calc R . .
H19B H 0.8495 0.7797 0.1811 0.091 Uiso 1 1 calc R . .
H19C H 0.8567 0.8155 0.2295 0.091 Uiso 1 1 calc R . .
C20 C 0.73533(10) 0.83096(9) 0.21414(7) 0.0388(4) Uani 1 1 d . . .
H20A H 0.7578 0.8704 0.2243 0.047 Uiso 1 1 calc R . .
C21 C 0.67689(10) 0.79931(9) 0.22773(7) 0.0369(4) Uani 1 1 d . . .
C22 C 0.65067(12) 0.82649(11) 0.25964(8) 0.0505(6) Uani 1 1 d . . .
H22A H 0.6128 0.8178 0.2466 0.076 Uiso 1 1 calc R . .
H22B H 0.6768 0.8688 0.2607 0.076 Uiso 1 1 calc R . .
H22C H 0.6455 0.8104 0.2923 0.076 Uiso 1 1 calc R . .
C23 C 0.64380(9) 0.74326(8) 0.21031(6) 0.0324(4) Uani 1 1 d . . .
H23A H 0.6035 0.7218 0.2180 0.039 Uiso 1 1 calc R . .
C24 C 0.63487(8) 0.64565(8) 0.10865(6) 0.0290(4) Uani 1 1 d . . .
C25 C 0.66661(8) 0.61967(8) 0.09388(6) 0.0307(4) Uani 1 1 d . . .
C26 C 0.66937(8) 0.60546(8) 0.04526(6) 0.0332(4) Uani 1 1 d . . .
C27 C 0.70243(10) 0.57398(10) 0.02988(7) 0.0419(5) Uani 1 1 d . . .
C28 C 0.76814(11) 0.61270(13) 0.03935(9) 0.0576(6) Uani 1 1 d . . .
H28A H 0.7750 0.6189 0.0741 0.086 Uiso 1 1 calc R . .
H28B H 0.7824 0.6503 0.0232 0.086 Uiso 1 1 calc R . .
H28C H 0.7888 0.5935 0.0267 0.086 Uiso 1 1 calc R . .
C29 C 0.67811(13) 0.51563(11) 0.05658(8) 0.0536(6) Uani 1 1 d . . .
H29A H 0.6836 0.5228 0.0913 0.080 Uiso 1 1 calc R . .
H29B H 0.6988 0.4956 0.0459 0.080 Uiso 1 1 calc R . .
H29C H 0.6365 0.4913 0.0495 0.080 Uiso 1 1 calc R . .
C30 C 0.69492(13) 0.56015(13) -0.02441(8) 0.0588(7) Uani 1 1 d . . .
H30A H 0.7091 0.5964 -0.0427 0.088 Uiso 1 1 calc R . .
H30B H 0.6536 0.5339 -0.0316 0.088 Uiso 1 1 calc R . .
H30C H 0.7173 0.5413 -0.0335 0.088 Uiso 1 1 calc R . .
C31 C 0.63947(9) 0.62018(8) 0.01213(7) 0.0369(4) Uani 1 1 d . . .
H31A H 0.6403 0.6111 -0.0209 0.044 Uiso 1 1 calc R . .
C32 C 0.60853(9) 0.64750(8) 0.02501(7) 0.0355(4) Uani 1 1 d . . .
C33 C 0.57643(11) 0.66245(11) -0.01243(8) 0.0487(5) Uani 1 1 d . . .
H33A H 0.5740 0.6964 -0.0016 0.073 Uiso 1 1 calc R . .
H33B H 0.5370 0.6292 -0.0167 0.073 Uiso 1 1 calc R . .
H33C H 0.5975 0.6714 -0.0431 0.073 Uiso 1 1 calc R . .
C34 C 0.60612(8) 0.65906(8) 0.07336(6) 0.0313(4) Uani 1 1 d . . .
H34A H 0.5841 0.6768 0.0827 0.038 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
O3 As1 O1 98.18(6) . . ?
O3 As1 O2 100.00(6) . . ?
O1 As1 O2 100.50(6) . . ?
C3 O1 As1 123.48(11) . . ?
C13 C1 C2 114.28(14) . . ?
C13 C1 C24 116.78(15) . . ?
C2 C1 C24 114.90(15) . . ?
C14 O2 As1 122.69(11) . . ?
C3 C2 C12 118.40(16) . . ?
C3 C2 C1 124.79(16) . . ?
C12 C2 C1 116.70(15) . . ?
C25 O3 As1 123.14(11) . . ?
C2 C3 O1 119.40(16) . . ?
C2 C3 C4 122.01(17) . . ?
O1 C3 C4 118.57(16) . . ?
C9 C4 C3 116.31(17) . . ?
C9 C4 C5 121.17(17) . . ?
C3 C4 C5 122.52(17) . . ?
C7 C5 C8 110.0(2) . . ?
C7 C5 C6 107.32(18) . . ?
C8 C5 C6 106.72(19) . . ?
C7 C5 C4 111.11(16) . . ?
C8 C5 C4 110.05(16) . . ?
C6 C5 C4 111.48(18) . . ?
C10 C9 C4 123.54(17) . . ?
C12 C10 C9 117.95(18) . . ?
C12 C10 C11 120.74(18) . . ?
C9 C10 C11 121.27(17) . . ?
C10 C12 C2 121.69(17) . . ?
C14 C13 C23 118.21(17) . . ?
C14 C13 C1 124.76(16) . . ?
C23 C13 C1 116.93(16) . . ?
C13 C14 O2 119.29(17) . . ?
C13 C14 C15 122.01(17) . . ?
O2 C14 C15 118.69(17) . . ?
C20 C15 C14 116.60(19) . . ?
C20 C15 C16 121.55(18) . . ?
C14 C15 C16 121.85(18) . . ?
C19 C16 C17 110.3(2) . . ?
C19 C16 C15 110.80(18) . . ?
C17 C16 C15 110.22(18) . . ?
C19 C16 C18 107.7(2) . . ?
C17 C16 C18 106.6(2) . . ?
C15 C16 C18 111.10(19) . . ?
C15 C20 C21 123.00(19) . . ?
C23 C21 C20 117.98(18) . . ?
C23 C21 C22 121.4(2) . . ?
C20 C21 C22 120.57(19) . . ?
C21 C23 C13 121.99(19) . . ?
C25 C24 C34 117.58(16) . . ?
C25 C24 C1 124.74(16) . . ?
C34 C24 C1 117.54(16) . . ?
C24 C25 O3 119.67(15) . . ?
C24 C25 C26 122.62(17) . . ?
O3 C25 C26 117.70(16) . . ?
C31 C26 C25 116.38(18) . . ?
C31 C26 C27 121.74(17) . . ?
C25 C26 C27 121.87(17) . . ?
C29 C27 C28 110.7(2) . . ?
C29 C27 C30 107.07(19) . . ?
C28 C27 C30 107.12(19) . . ?
C29 C27 C26 110.19(17) . . ?
C28 C27 C26 110.60(18) . . ?
C30 C27 C26 111.03(18) . . ?
C32 C31 C26 123.02(18) . . ?
C31 C32 C34 118.07(18) . . ?
C31 C32 C33 121.05(18) . . ?
C34 C32 C33 120.85(19) . . ?
C32 C34 C24 122.29(18) . . ?
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
As1 O3 1.7724(13) . ?
As1 O1 1.7756(12) . ?
As1 O2 1.7850(13) . ?
O1 C3 1.395(2) . ?
C1 C13 1.526(3) . ?
C1 C2 1.529(2) . ?
C1 C24 1.539(2) . ?
O2 C14 1.392(2) . ?
C2 C3 1.389(2) . ?
C2 C12 1.399(3) . ?
O3 C25 1.398(2) . ?
C3 C4 1.412(3) . ?
C4 C9 1.389(3) . ?
C4 C5 1.539(3) . ?
C5 C7 1.533(3) . ?
C5 C8 1.535(3) . ?
C5 C6 1.537(3) . ?
C9 C10 1.388(3) . ?
C10 C12 1.380(3) . ?
C10 C11 1.508(3) . ?
C13 C14 1.387(3) . ?
C13 C23 1.395(3) . ?
C14 C15 1.417(3) . ?
C15 C20 1.388(3) . ?
C15 C16 1.542(3) . ?
C16 C19 1.534(4) . ?
C16 C17 1.540(3) . ?
C16 C18 1.550(3) . ?
C20 C21 1.394(3) . ?
C21 C23 1.381(3) . ?
C21 C22 1.512(3) . ?
C24 C25 1.388(3) . ?
C24 C34 1.392(2) . ?
C25 C26 1.413(2) . ?
C26 C31 1.391(3) . ?
C26 C27 1.541(3) . ?
C27 C29 1.536(3) . ?
C27 C28 1.538(3) . ?
C27 C30 1.540(3) . ?
C31 C32 1.384(3) . ?
C32 C34 1.385(3) . ?
C32 C33 1.516(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661078
