#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:20:11 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191457 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/93/7119398.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_7119398
loop_
_publ_author_name
'Gao, Chao-Ying'
'Ai, Jing'
'Tian, Hong-Rui'
'Wu, Dai'
'Sun, Zhong-Ming'
_publ_section_title
;
 An ultrastable zirconium-phosphonate framework as bifunctional catalyst
 for highly active CO2 chemical transformation.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1293
_journal_page_last               1296
_journal_paper_doi               10.1039/c6cc08773f
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C24 H20 O12 P4 Si Zr'
_chemical_formula_sum            'C24 H20 N0 O12 P4 Si Zr'
_chemical_formula_weight         743.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_audit_update_record
;
2016-09-04 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.702(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9688(2)
_cell_length_b                   19.2157(4)
_cell_length_c                   14.5392(3)
_cell_measurement_reflns_used    5132
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.22
_cell_measurement_theta_min      3.85
_cell_volume                     2745.26(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10653
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.217
_diffrn_reflns_theta_min         3.848
_exptl_absorpt_coefficient_mu    6.500
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.186
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0893P)²+1.8272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4030
_reflns_number_total             5132
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc08773f2.cif
_cod_data_source_block           zr_sq
_cod_depositor_comments          'Adding full bibliography for 7119398.cif.'
_cod_original_cell_volume        2745.26(11)
_cod_database_code               7119398
_shelxl_version_number           2014-3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.263
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6A), C8(H8), C9(H9), C11(H11), C12(H12A),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H6), O12(H12), O9(H9A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Zr1 Zr 0.74982(2) 0.54975(2) 0.49874(2) 0.01610(14) Uani 1 1 d .
Si1 Si 0.26115(9) 0.89556(6) 0.49988(6) 0.0221(2) Uani 1 1 d .
P1 P -0.01975(9) 1.05923(5) 0.12781(6) 0.0184(2) Uani 1 1 d .
P2 P -0.18317(10) 0.69504(5) 0.64500(7) 0.0269(2) Uani 1 1 d .
P3 P 0.67869(11) 0.68638(5) 0.34157(7) 0.0269(2) Uani 1 1 d .
P4 P 0.52163(9) 1.06219(5) 0.87352(6) 0.0182(2) Uani 1 1 d .
O1 O -0.0425(3) 1.13736(15) 0.1467(2) 0.0286(6) Uani 1 1 d .
H1 H 0.0289 1.1587 0.1472 0.043 Uiso 1 1 calc GR
O2 O 0.0781(3) 1.05098(14) 0.05973(19) 0.0246(6) Uani 1 1 d .
O3 O -0.1556(3) 1.02543(14) 0.09159(17) 0.0211(5) Uani 1 1 d .
O4 O -0.3253(3) 0.72463(17) 0.6325(2) 0.0363(7) Uani 1 1 d .
O6 O -0.1282(3) 0.67674(17) 0.7493(2) 0.0356(7) Uani 1 1 d .
H6 H -0.1476 0.7081 0.7829 0.053 Uiso 1 1 calc GR
O7 O 0.8204(3) 0.71582(16) 0.3491(2) 0.0343(7) Uani 1 1 d .
O8 O 0.6709(3) 0.61851(15) 0.3949(2) 0.0294(6) Uani 1 1 d .
O10 O 0.4182(3) 1.05308(14) 0.93803(19) 0.0241(6) Uani 1 1 d .
O11 O 0.6582(3) 1.03012(14) 0.91234(17) 0.0209(5) Uani 1 1 d .
O12 O 0.5430(3) 1.14126(14) 0.8580(2) 0.0288(6) Uani 1 1 d .
H12 H 0.4727 1.1624 0.8618 0.043 Uiso 1 1 calc GR
C1 C 0.1812(4) 0.9481(2) 0.3957(3) 0.0258(8) Uani 1 1 d .
C2 C 0.1511(5) 1.0184(2) 0.3975(3) 0.0355(9) Uani 1 1 d .
H2 H 0.1731 1.0429 0.4532 0.043 Uiso 1 1 calc R
C3 C 0.0888(5) 1.0533(2) 0.3177(3) 0.0337(9) Uani 1 1 d .
H3 H 0.0686 1.1004 0.3206 0.040 Uiso 1 1 calc R
C4 C 0.0569(4) 1.0178(2) 0.2342(2) 0.0219(7) Uani 1 1 d .
C5 C 0.0907(5) 0.9474(2) 0.2299(3) 0.0404(11) Uani 1 1 d .
H5 H 0.0715 0.9233 0.1737 0.048 Uiso 1 1 calc R
C6 C 0.1529(5) 0.9139(2) 0.3102(3) 0.0395(10) Uani 1 1 d .
H6A H 0.1764 0.8673 0.3069 0.047 Uiso 1 1 calc R
C7 C 0.1283(4) 0.8420(2) 0.5438(3) 0.0272(8) Uani 1 1 d .
C8 C -0.0053(5) 0.8394(3) 0.4993(3) 0.0370(9) Uani 1 1 d .
H8 H -0.0321 0.8663 0.4461 0.044 Uiso 1 1 calc R
C9 C -0.1011(5) 0.7975(3) 0.5323(3) 0.0383(10) Uani 1 1 d .
H9 H -0.1909 0.7978 0.5018 0.046 Uiso 1 1 calc R
C10 C -0.0639(4) 0.7553(2) 0.6099(3) 0.0287(8) Uani 1 1 d .
C11 C 0.0702(5) 0.7593(3) 0.6565(4) 0.0448(11) Uani 1 1 d .
H11 H 0.0970 0.7325 0.7097 0.054 Uiso 1 1 calc R
C12 C 0.1636(5) 0.8022(3) 0.6252(3) 0.0451(12) Uani 1 1 d .
H12A H 0.2516 0.8048 0.6586 0.054 Uiso 1 1 calc R
C13 C 0.3857(4) 0.8348(2) 0.4582(3) 0.0266(8) Uani 1 1 d .
C14 C 0.3655(5) 0.7628(3) 0.4557(4) 0.0463(12) Uani 1 1 d .
H14 H 0.2917 0.7442 0.4788 0.056 Uiso 1 1 calc R
C15 C 0.4536(5) 0.7183(3) 0.4194(4) 0.0475(12) Uani 1 1 d .
H15 H 0.4381 0.6706 0.4178 0.057 Uiso 1 1 calc R
C16 C 0.5650(4) 0.7456(2) 0.3854(3) 0.0300(8) Uani 1 1 d .
C17 C 0.5850(5) 0.8154(2) 0.3851(3) 0.0359(9) Uani 1 1 d .
H17 H 0.6576 0.8335 0.3602 0.043 Uiso 1 1 calc R
C18 C 0.4976(5) 0.8600(2) 0.4218(3) 0.0366(9) Uani 1 1 d .
H18 H 0.5140 0.9077 0.4221 0.044 Uiso 1 1 calc R
C19 C 0.3434(4) 0.95138(19) 0.5991(3) 0.0239(8) Uani 1 1 d .
C20 C 0.4836(4) 0.9499(2) 0.6333(3) 0.0315(9) Uani 1 1 d .
H20 H 0.5411 0.9259 0.6002 0.038 Uiso 1 1 calc R
C21 C 0.5388(4) 0.9839(2) 0.7162(3) 0.0313(8) Uani 1 1 d .
H21 H 0.6316 0.9813 0.7390 0.038 Uiso 1 1 calc R
C22 C 0.4538(4) 1.0216(2) 0.7643(2) 0.0225(7) Uani 1 1 d .
C23 C 0.3164(4) 1.0265(2) 0.7296(3) 0.0304(8) Uani 1 1 d .
H23 H 0.2602 1.0530 0.7608 0.036 Uiso 1 1 calc R
C24 C 0.2624(4) 0.9918(2) 0.6482(3) 0.0321(9) Uani 1 1 d .
H24 H 0.1697 0.9955 0.6255 0.039 Uiso 1 1 calc R
O5 O -0.1736(3) 0.62781(15) 0.5894(2) 0.0295(6) Uani 1 1 d .
O9 O 0.6171(4) 0.67163(17) 0.2377(2) 0.0378(7) Uani 1 1 d .
H9A H 0.6326 0.7047 0.2054 0.057 Uiso 1 1 calc GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
O2 Zr1 O3 87.56(10) 2_645 4_676
O2 Zr1 O8 86.04(11) 2_645 .
O2 Zr1 O10 176.79(11) 2_645 2_646
O2 Zr1 O11 94.05(10) 2_645 4_575
O2 Zr1 O5 90.64(11) 2_645 1_655
O3 Zr1 O11 89.11(12) 4_676 4_575
O8 Zr1 O3 172.52(11) . 4_676
O8 Zr1 O11 87.49(11) . 4_575
O10 Zr1 O3 92.63(10) 2_646 4_676
O10 Zr1 O8 93.98(11) 2_646 .
O10 Zr1 O11 89.16(10) 2_646 4_575
O10 Zr1 O5 86.15(11) 2_646 1_655
O5 Zr1 O3 90.68(12) 1_655 4_676
O5 Zr1 O8 93.25(13) 1_655 .
O5 Zr1 O11 175.29(10) 1_655 4_575
C7 Si1 C1 109.93(19) . .
C7 Si1 C13 108.2(2) . .
C13 Si1 C1 106.70(18) . .
C19 Si1 C1 112.58(19) . .
C19 Si1 C7 107.20(18) . .
C19 Si1 C13 112.17(19) . .
O1 P1 C4 109.36(17) . .
O2 P1 O1 110.34(16) . .
O2 P1 O3 111.43(16) . .
O2 P1 C4 106.88(17) . .
O3 P1 O1 109.16(16) . .
O3 P1 C4 109.63(16) . .
O4 P2 O6 111.77(18) . .
O4 P2 C10 112.1(2) . .
O4 P2 O5 113.18(17) . .
O6 P2 C10 106.25(19) . .
O5 P2 O6 106.19(18) . .
O5 P2 C10 106.89(18) . .
O7 P3 O8 114.25(17) . .
O7 P3 C16 112.0(2) . .
O7 P3 O9 110.49(19) . .
O8 P3 C16 105.83(18) . .
O8 P3 O9 106.95(18) . .
O9 P3 C16 106.8(2) . .
O10 P4 O12 109.07(16) . .
O10 P4 C22 107.63(17) . .
O11 P4 O10 112.65(15) . .
O11 P4 O12 108.35(16) . .
O11 P4 C22 109.51(16) . .
O12 P4 C22 109.61(17) . .
P1 O2 Zr1 162.94(19) . 2_655
P1 O3 Zr1 143.22(16) . 4_475
P3 O8 Zr1 151.01(19) . .
P4 O10 Zr1 167.55(19) . 2_656
P4 O11 Zr1 142.74(16) . 4_576
C2 C1 Si1 124.9(3) . .
C2 C1 C6 117.6(4) . .
C6 C1 Si1 117.4(3) . .
C1 C2 C3 121.5(4) . .
C4 C3 C2 119.9(4) . .
C3 C4 P1 122.7(3) . .
C3 C4 C5 119.7(4) . .
C5 C4 P1 117.5(3) . .
C6 C5 C4 119.2(4) . .
C5 C6 C1 121.9(4) . .
C8 C7 Si1 122.8(3) . .
C8 C7 C12 117.4(4) . .
C12 C7 Si1 119.7(3) . .
C7 C8 C9 121.5(4) . .
C10 C9 C8 120.8(4) . .
C9 C10 P2 120.6(3) . .
C9 C10 C11 117.8(4) . .
C11 C10 P2 121.6(3) . .
C12 C11 C10 121.1(4) . .
C11 C12 C7 121.2(4) . .
C14 C13 Si1 121.6(3) . .
C14 C13 C18 117.0(4) . .
C18 C13 Si1 121.3(3) . .
C15 C14 C13 121.4(4) . .
C14 C15 C16 119.6(4) . .
C15 C16 P3 118.4(3) . .
C17 C16 P3 121.6(3) . .
C17 C16 C15 120.1(4) . .
C16 C17 C18 120.5(4) . .
C17 C18 C13 121.4(4) . .
C20 C19 Si1 122.9(3) . .
C24 C19 Si1 119.7(3) . .
C24 C19 C20 117.2(4) . .
C21 C20 C19 121.3(4) . .
C22 C21 C20 119.5(4) . .
C21 C22 P4 120.0(3) . .
C23 C22 P4 119.7(3) . .
C23 C22 C21 120.2(4) . .
C22 C23 C24 119.9(4) . .
C23 C24 C19 121.9(4) . .
P2 O5 Zr1 154.38(19) . 1_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O2 2.039(3) 2_645
Zr1 O3 2.090(3) 4_676
Zr1 O8 2.060(3) .
Zr1 O10 2.043(3) 2_646
Zr1 O11 2.093(3) 4_575
Zr1 O5 2.057(3) 1_655
Si1 C1 1.881(4) .
Si1 C7 1.872(4) .
Si1 C13 1.878(4) .
Si1 C19 1.872(4) .
P1 O1 1.550(3) .
P1 O2 1.511(3) .
P1 O3 1.514(3) .
P1 C4 1.792(4) .
P2 O4 1.509(3) .
P2 O6 1.563(3) .
P2 C10 1.795(4) .
P2 O5 1.536(3) .
P3 O7 1.508(3) .
P3 O8 1.525(3) .
P3 C16 1.797(4) .
P3 O9 1.558(3) .
P4 O10 1.517(3) .
P4 O11 1.514(3) .
P4 O12 1.556(3) .
P4 C22 1.796(4) .
O2 Zr1 2.039(3) 2_655
O3 Zr1 2.090(3) 4_475
O10 Zr1 2.043(3) 2_656
O11 Zr1 2.093(3) 4_576
C1 C2 1.386(6) .
C1 C6 1.393(6) .
C2 C3 1.392(6) .
C3 C4 1.382(5) .
C4 C5 1.399(6) .
C5 C6 1.384(6) .
C7 C8 1.380(6) .
C7 C12 1.404(6) .
C8 C9 1.394(6) .
C9 C10 1.388(6) .
C10 C11 1.395(6) .
C11 C12 1.377(6) .
C13 C14 1.397(7) .
C13 C18 1.401(6) .
C14 C15 1.392(7) .
C15 C16 1.393(7) .
C16 C17 1.355(6) .
C17 C18 1.392(6) .
C19 C20 1.403(6) .
C19 C24 1.400(6) .
C20 C21 1.400(6) .
C21 C22 1.390(6) .
C22 C23 1.381(6) .
C23 C24 1.386(6) .
O5 Zr1 2.057(3) 1_455
