#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:02:55 +0300 (Fri, 06 May 2016) $
#$Revision: 182664 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/88/7038890.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_7038890
loop_
_publ_author_name
'Chatterjee, Tamal'
'Lee, Way-Zen'
'Ravikanth, Mangalampalli'
_publ_section_title
;
 Stabilization of hexa-coordinated P(v) corroles by axial silyloxy groups.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7815
_journal_page_last               7822
_journal_paper_doi               10.1039/c6dt00842a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C69 H61 N4 O2 P Si2'
_chemical_formula_sum            'C69 H61 N4 O2 P Si2'
_chemical_formula_weight         1065.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-16 deposited with the CCDC.
2016-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.414(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6832(7)
_cell_length_b                   14.4882(9)
_cell_length_c                   23.4948(15)
_cell_measurement_reflns_used    6574
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.44
_cell_volume                     5677.2(6)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'bruker APEX2'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17286
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9483
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4894
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0702
_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)+(0.0638P)²+30.5253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                3816
_reflns_number_total             4894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00842a2.cif
_cod_data_source_block           a17648
_cod_depositor_comments          'Adding full bibliography for 7038890.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7038890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.7628(2) 0.1220(3) 0.82262(16) 0.0361(9) Uani 1 1 d .
C2 C 0.7405(2) 0.0698(4) 0.76779(16) 0.0480(12) Uani 1 1 d .
H2A H 0.7790 0.0849 0.7384 0.072 Uiso 1 1 calc R
H2B H 0.6865 0.0878 0.7547 0.072 Uiso 1 1 calc R
H2C H 0.7418 0.0033 0.7752 0.072 Uiso 1 1 calc R
C3 C 0.7577(3) 0.2264(4) 0.8101(3) 0.0668(15) Uani 1 1 d .
H3A H 0.7967 0.2426 0.7811 0.100 Uiso 1 1 calc R
H3B H 0.7698 0.2611 0.8450 0.100 Uiso 1 1 calc R
H3C H 0.7036 0.2418 0.7960 0.100 Uiso 1 1 calc R
C4 C 0.7021(2) 0.0965(4) 0.86830(18) 0.0556(14) Uani 1 1 d .
H4A H 0.7160 0.1288 0.9038 0.083 Uiso 1 1 calc R
H4B H 0.7035 0.0297 0.8748 0.083 Uiso 1 1 calc R
H4C H 0.6481 0.1148 0.8553 0.083 Uiso 1 1 calc R
C5 C 0.8902(2) 0.1744(3) 0.91207(15) 0.0293(8) Uani 1 1 d .
C6 C 0.9389(2) 0.2523(3) 0.90787(17) 0.0374(9) Uani 1 1 d .
H6 H 0.9660 0.2636 0.8735 0.045 Uiso 1 1 calc R
C7 C 0.9487(3) 0.3138(3) 0.95308(19) 0.0473(11) Uani 1 1 d .
H7 H 0.9836 0.3652 0.9497 0.057 Uiso 1 1 calc R
C8 C 0.9079(3) 0.3003(3) 1.00269(18) 0.0486(11) Uani 1 1 d .
H8 H 0.9130 0.3436 1.0329 0.058 Uiso 1 1 calc R
C9 C 0.8597(3) 0.2238(3) 1.00820(17) 0.0448(11) Uani 1 1 d .
H9 H 0.8317 0.2140 1.0424 0.054 Uiso 1 1 calc R
C10 C 0.8519(2) 0.1606(3) 0.96372(16) 0.0380(9) Uani 1 1 d .
H10 H 0.8199 0.1070 0.9685 0.046 Uiso 1 1 calc R
C11 C 0.8876(2) -0.0253(3) 0.87168(15) 0.0290(8) Uani 1 1 d .
C12 C 0.9385(2) -0.0429(3) 0.91836(17) 0.0367(9) Uani 1 1 d .
H12 H 0.9631 0.0077 0.9377 0.044 Uiso 1 1 calc R
C13 C 0.9543(3) -0.1321(3) 0.93747(19) 0.0470(11) Uani 1 1 d .
H13 H 0.9894 -0.1420 0.9694 0.056 Uiso 1 1 calc R
C14 C 0.9189(3) -0.2064(3) 0.9098(2) 0.0513(12) Uani 1 1 d .
H14 H 0.9290 -0.2675 0.9228 0.062 Uiso 1 1 calc R
C15 C 0.8688(3) -0.1915(3) 0.8630(2) 0.0491(11) Uani 1 1 d .
H15 H 0.8447 -0.2425 0.8438 0.059 Uiso 1 1 calc R
C16 C 0.8535(2) -0.1024(3) 0.84392(18) 0.0384(9) Uani 1 1 d .
H16 H 0.8193 -0.0933 0.8115 0.046 Uiso 1 1 calc R
C17 C 0.9712(2) -0.0586(2) 0.72767(15) 0.0255(7) Uani 1 1 d .
C18 C 0.9285(2) -0.1216(3) 0.69299(16) 0.0312(8) Uani 1 1 d .
H18 H 0.9315 -0.1870 0.6948 0.037 Uiso 1 1 calc R
C19 C 0.8815(2) -0.0703(3) 0.65591(16) 0.0321(9) Uani 1 1 d .
H19 H 0.8463 -0.0943 0.6271 0.039 Uiso 1 1 calc R
C20 C 0.8944(2) 0.0245(2) 0.66808(14) 0.0243(8) Uani 1 1 d .
C21 C 0.8611(2) 0.1038(2) 0.64398(14) 0.0258(8) Uani 1 1 d .
C22 C 0.7991(2) 0.0950(3) 0.59733(15) 0.0303(8) Uani 1 1 d .
C23 C 0.8126(3) 0.1309(3) 0.5436(2) 0.0533(9) Uani 1 1 d .
H23 H 0.8607 0.1636 0.5368 0.064 Uiso 1 1 calc R
C24 C 0.7560(3) 0.1193(4) 0.4995(3) 0.0766(13) Uani 1 1 d .
H24 H 0.7661 0.1437 0.4628 0.092 Uiso 1 1 calc R
C25 C 0.6860(3) 0.0731(4) 0.5088(3) 0.0735(14) Uani 1 1 d .
H25 H 0.6472 0.0660 0.4788 0.088 Uiso 1 1 calc R
C26 C 0.6721(3) 0.0368(4) 0.5620(2) 0.0599(14) Uani 1 1 d .
H26 H 0.6238 0.0043 0.5684 0.072 Uiso 1 1 calc R
C27 C 0.7281(3) 0.0474(3) 0.60587(18) 0.0463(11) Uani 1 1 d .
H27 H 0.7179 0.0219 0.6422 0.056 Uiso 1 1 calc R
C28 C 0.8843(2) 0.1902(2) 0.66446(14) 0.0247(8) Uani 1 1 d .
C29 C 0.8520(2) 0.2765(3) 0.64595(15) 0.0299(8) Uani 1 1 d .
H29 H 0.8111 0.2846 0.6175 0.036 Uiso 1 1 calc R
C30 C 0.8892(2) 0.3450(3) 0.67556(15) 0.0294(8) Uani 1 1 d .
H30 H 0.8791 0.4092 0.6716 0.035 Uiso 1 1 calc R
C31 C 0.94648(19) 0.3031(2) 0.71375(14) 0.0246(8) Uani 1 1 d .
C32 C 1.0000 0.3495(3) 0.7500 0.0266(11) Uani 1 2 d S
C33 C 1.0000 0.4523(4) 0.7500 0.0429(15) Uani 1 2 d SDU
C34 C 0.9757(3) 0.5005(3) 0.7975(2) 0.0533(9) Uani 1 1 d DU
H34 H 0.9587 0.4683 0.8303 0.064 Uiso 1 1 calc R
C35 C 0.9765(3) 0.5990(4) 0.7967(3) 0.0766(13) Uani 1 1 d DU
H35 H 0.9607 0.6342 0.8287 0.092 Uiso 1 1 calc R
C36 C 1.0000 0.6387(6) 0.7500 0.0735(14) Uani 1 2 d SDU
H36 H 1.0000 0.7043 0.7500 0.088 Uiso 1 2 calc SR
N1 N 0.94994(16) 0.02920(19) 0.71217(11) 0.0224(6) Uani 1 1 d .
N2 N 0.94243(15) 0.20835(19) 0.70753(11) 0.0219(6) Uani 1 1 d .
O1 O 0.92863(13) 0.12820(16) 0.79761(9) 0.0247(5) Uani 1 1 d .
Si1 Si 0.86962(5) 0.09746(7) 0.84861(4) 0.0240(3) Uani 1 1 d .
P1 P 1.0000 0.12323(8) 0.7500 0.0196(3) Uani 1 2 d S
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'
N N 0.0061 0.0033 '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'
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
C2 C1 C4 108.5(3) . .
C2 C1 C3 108.2(4) . .
C4 C1 C3 109.6(4) . .
C2 C1 Si1 112.5(3) . .
C4 C1 Si1 111.0(3) . .
C3 C1 Si1 106.9(3) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 C10 117.1(3) . .
C6 C5 Si1 121.1(3) . .
C10 C5 Si1 121.5(3) . .
C7 C6 C5 121.4(4) . .
C7 C6 H6 119.3 . .
C5 C6 H6 119.3 . .
C8 C7 C6 120.2(4) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C9 C8 C7 119.7(4) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 120.2(4) . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C9 C10 C5 121.4(4) . .
C9 C10 H10 119.3 . .
C5 C10 H10 119.3 . .
C12 C11 C16 116.9(4) . .
C12 C11 Si1 119.3(3) . .
C16 C11 Si1 123.9(3) . .
C13 C12 C11 122.0(4) . .
C13 C12 H12 119.0 . .
C11 C12 H12 119.0 . .
C14 C13 C12 119.7(4) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C15 C14 C13 119.7(4) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C14 C15 C16 120.4(4) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C15 C16 C11 121.3(4) . .
C15 C16 H16 119.4 . .
C11 C16 H16 119.4 . .
N1 C17 C17 111.53(18) . 2_756
N1 C17 C18 108.9(3) . .
C17 C17 C18 139.5(2) 2_756 .
C19 C18 C17 106.8(3) . .
C19 C18 H18 126.6 . .
C17 C18 H18 126.6 . .
C18 C19 C20 108.3(3) . .
C18 C19 H19 125.9 . .
C20 C19 H19 125.9 . .
N1 C20 C21 121.4(3) . .
N1 C20 C19 107.3(3) . .
C21 C20 C19 131.4(3) . .
C20 C21 C28 119.9(3) . .
C20 C21 C22 119.4(3) . .
C28 C21 C22 120.8(3) . .
C27 C22 C23 118.3(3) . .
C27 C22 C21 120.9(3) . .
C23 C22 C21 120.7(3) . .
C22 C23 C24 120.6(5) . .
C22 C23 H23 119.7 . .
C24 C23 H23 119.7 . .
C25 C24 C23 120.4(6) . .
C25 C24 H24 119.8 . .
C23 C24 H24 119.8 . .
C24 C25 C26 119.5(4) . .
C24 C25 H25 120.2 . .
C26 C25 H25 120.2 . .
C25 C26 C27 120.5(4) . .
C25 C26 H26 119.7 . .
C27 C26 H26 119.7 . .
C26 C27 C22 120.7(4) . .
C26 C27 H27 119.7 . .
C22 C27 H27 119.7 . .
C21 C28 N2 126.6(3) . .
C21 C28 C29 125.7(3) . .
N2 C28 C29 107.7(3) . .
C30 C29 C28 108.7(3) . .
C30 C29 H29 125.6 . .
C28 C29 H29 125.6 . .
C29 C30 C31 107.6(3) . .
C29 C30 H30 126.2 . .
C31 C30 H30 126.2 . .
N2 C31 C32 125.0(3) . .
N2 C31 C30 109.0(3) . .
C32 C31 C30 126.0(3) . .
C31 C32 C31 122.2(5) . 2_756
C31 C32 C33 118.9(2) . .
C31 C32 C33 118.9(2) 2_756 .
C34 C33 C34 119.4(6) 2_756 .
C34 C33 C32 120.3(3) 2_756 .
C34 C33 C32 120.3(3) . .
C33 C34 C35 119.4(5) . .
C33 C34 H34 120.3 . .
C35 C34 H34 120.3 . .
C36 C35 C34 116.9(6) . .
C36 C35 H35 121.5 . .
C34 C35 H35 121.5 . .
C35 C36 C35 127.9(9) 2_756 .
C35 C36 H36 116.1 2_756 .
C35 C36 H36 116.1 . .
C17 N1 C20 108.7(3) . .
C17 N1 P1 117.0(2) . .
C20 N1 P1 134.3(2) . .
C31 N2 C28 107.0(3) . .
C31 N2 P1 125.8(2) . .
C28 N2 P1 127.2(2) . .
Si1 O1 P1 160.33(17) . .
O1 Si1 C11 112.02(14) . .
O1 Si1 C5 108.52(15) . .
C11 Si1 C5 107.84(16) . .
O1 Si1 C1 106.89(15) . .
C11 Si1 C1 114.24(17) . .
C5 Si1 C1 107.10(17) . .
O1 P1 O1 175.01(18) 2_756 .
O1 P1 N1 91.81(12) 2_756 .
O1 P1 N1 91.93(12) . .
O1 P1 N1 91.93(12) 2_756 2_756
O1 P1 N1 91.81(12) . 2_756
N1 P1 N1 82.96(18) . 2_756
O1 P1 N2 88.79(12) 2_756 .
O1 P1 N2 87.87(12) . .
N1 P1 N2 90.56(12) . .
N1 P1 N2 173.50(13) 2_756 .
O1 P1 N2 87.87(12) 2_756 2_756
O1 P1 N2 88.79(12) . 2_756
N1 P1 N2 173.50(13) . 2_756
N1 P1 N2 90.56(12) 2_756 2_756
N2 P1 N2 95.92(17) . 2_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.531(6) .
C1 C4 1.538(6) .
C1 C3 1.543(6) .
C1 Si1 1.904(4) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.396(5) .
C5 C10 1.400(5) .
C5 Si1 1.886(4) .
C6 C7 1.393(5) .
C6 H6 0.9500 .
C7 C8 1.378(6) .
C7 H7 0.9500 .
C8 C9 1.378(6) .
C8 H8 0.9500 .
C9 C10 1.393(6) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.393(5) .
C11 C16 1.406(5) .
C11 Si1 1.881(4) .
C12 C13 1.392(6) .
C12 H12 0.9500 .
C13 C14 1.383(7) .
C13 H13 0.9500 .
C14 C15 1.381(7) .
C14 H14 0.9500 .
C15 C16 1.389(6) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 N1 1.368(4) .
C17 C17 1.404(7) 2_756
C17 C18 1.406(5) .
C18 C19 1.376(5) .
C18 H18 0.9500 .
C19 C20 1.418(5) .
C19 H19 0.9500 .
C20 N1 1.374(4) .
C20 C21 1.391(5) .
C21 C28 1.392(5) .
C21 C22 1.494(5) .
C22 C27 1.389(5) .
C22 C23 1.390(6) .
C23 C24 1.394(6) .
C23 H23 0.9500 .
C24 C25 1.368(9) .
C24 H24 0.9500 .
C25 C26 1.381(8) .
C25 H25 0.9500 .
C26 C27 1.383(6) .
C26 H26 0.9500 .
C27 H27 0.9500 .
C28 N2 1.409(4) .
C28 C29 1.425(5) .
C29 C30 1.354(5) .
C29 H29 0.9500 .
C30 C31 1.429(5) .
C30 H30 0.9500 .
C31 N2 1.383(4) .
C31 C32 1.392(4) .
C32 C31 1.392(4) 2_756
C32 C33 1.489(7) .
C33 C34 1.385(5) 2_756
C33 C34 1.385(5) .
C34 C35 1.428(7) .
C34 H34 0.9500 .
C35 C36 1.308(7) .
C35 H35 0.9500 .
C36 C35 1.308(7) 2_756
C36 H36 0.9500 .
N1 P1 1.818(3) .
N2 P1 1.842(3) .
O1 Si1 1.631(2) .
O1 P1 1.655(2) .
P1 O1 1.655(2) 2_756
P1 N1 1.818(3) 2_756
P1 N2 1.842(3) 2_756
