#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/67/7036757.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_7036757
loop_
_publ_author_name
'Begum, S.'
'Horike, S.'
'Kitagawa, S.'
'Krautscheid, H.'
_publ_section_title
;
 Water stable triazolyl phosphonate MOFs: steep water uptake and facile
 regeneration.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18727
_journal_page_last               18730
_journal_paper_doi               10.1039/c5dt02651b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'Co4 3(C8 H6 N3 P O3), O H, 15(H2 O), 0.5(S O4)'
_chemical_formula_sum            'C24 H49 Co4 N9 O27 P3 S0.5'
_chemical_formula_weight         1240.38
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-07 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   20.5940(16)
_cell_length_b                   20.5940(16)
_cell_length_c                   6.5304(4)
_cell_measurement_reflns_used    4345
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.0
_cell_volume                     2398.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'DIAMOND 3.2e'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS  2T'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         1.145
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1266
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.638
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1465
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0913P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1176
_reflns_number_total             1465
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02651b2.cif
_cod_data_source_block           ip2-2085
_cod_depositor_comments          'Adding full bibliography for 7036757.cif.'
_cod_original_cell_volume        2398.6(4)
_cod_original_formula_sum        'C24 H49 Co4 N9 O27 P3 S0.50'
_cod_database_code               7036757
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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_min   0.708
_shelx_estimated_absorpt_t_max   0.941
_platon_squeeze_void_probe_radius 1.20
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'y, x, z+1/2'
'-x, -x+y, z+1/2'
'x-y, -y, z+1/2'
'x, y, -z+1/2'
'-x+y, -x, -z+1/2'
'-y, x-y, -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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.55508(11) 0.30242(11) 0.7500 0.0188(5) Uani 1 2 d S T P
Co2 Co 0.6667 0.3333 0.2500 0.0688(17) Uani 1 6 d S T P
O1 O 0.6667 0.3333 0.684(3) 0.025(6) Uiso 0.5 3 d S . P
H1 H 0.6667 0.3333 0.5551 0.029 Uiso 0.5 3 calc R U P
O4 O 0.4439(9) 0.2769(8) 0.8080(19) 0.037(4) Uiso 0.5 1 d . . P
C1 C 0.4703(7) 0.1654(8) 0.2500 0.022(3) Uani 1 2 d S TU P
C2 C 0.3968(8) 0.1105(7) 0.2500 0.017(3) Uani 1 2 d S T P
H2 H 0.3596 0.1250 0.2500 0.020 Uiso 1 2 calc R U P
C3 C 0.3737(7) 0.0352(8) 0.2500 0.024(3) Uani 1 2 d S T P
H3 H 0.3220 -0.0016 0.2500 0.029 Uiso 1 2 calc R U P
C4 C 0.4299(7) 0.0143(6) 0.2500 0.013(3) Uani 1 2 d S T P
C5 C 0.5023(11) 0.0682(11) 0.2500 0.037(4) Uani 1 2 d S T P
H5 H 0.5394 0.0536 0.2500 0.044 Uiso 1 2 calc R U P
C6 C 0.5254(9) 0.1427(9) 0.2500 0.028(3) Uani 1 2 d S T P
H6 H 0.5773 0.1791 0.2500 0.033 Uiso 1 2 calc R U P
C7 C 0.3379(8) -0.1249(7) 0.2500 0.021(3) Uani 1 2 d S T P
H7 H 0.2937 -0.1213 0.2500 0.026 Uiso 1 2 calc R U P
C8 C 0.4508(8) -0.0955(8) 0.2500 0.020(3) Uani 1 2 d S T P
H8 H 0.5041 -0.0674 0.2500 0.024 Uiso 1 2 calc R U P
N1 N 0.4067(7) -0.0655(6) 0.2500 0.019(3) Uani 1 2 d S T P
N2 N 0.3374(7) -0.1879(6) 0.2500 0.017(2) Uani 1 2 d S T P
N3 N 0.4112(6) -0.1689(6) 0.2500 0.017(2) Uani 1 2 d S T P
P1 P 0.5040(3) 0.2634(2) 0.2500 0.0358(12) Uani 1 2 d S T P
O2A O 0.5647(6) 0.2983(6) 0.4300(12) 0.0234(19) Uiso 0.65 1 d . . P
O2B O 0.5283(11) 0.3029(10) 0.449(2) 0.022(4) Uiso 0.35 1 d . . P
O3 O 0.4338(10) 0.2710(9) 0.288(4) 0.065(6) Uiso 0.5 1 d . . P
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
O2B Co1 O2B 148.3(11) . 10_556
O2B Co1 O1 117.0(7) . 10_556
O2B Co1 O1 93.3(8) 10_556 10_556
O2B Co1 O1 93.3(8) . .
O2B Co1 O1 117.0(7) 10_556 .
O1 Co1 O1 23.8(10) 10_556 .
O2B Co1 O2A 170.6(7) . 10_556
O2B Co1 O2A 22.5(5) 10_556 10_556
O1 Co1 O2A 72.4(6) 10_556 10_556
O1 Co1 O2A 96.1(6) . 10_556
O2B Co1 O2A 22.5(5) . .
O2B Co1 O2A 170.6(7) 10_556 .
O1 Co1 O2A 96.1(6) 10_556 .
O1 Co1 O2A 72.4(6) . .
O2A Co1 O2A 166.3(6) 10_556 .
O2B Co1 O4 64.3(7) . 10_556
O2B Co1 O4 84.9(7) 10_556 10_556
O1 Co1 O4 176.7(5) 10_556 10_556
O1 Co1 O4 157.6(6) . 10_556
O2A Co1 O4 106.3(4) 10_556 10_556
O2A Co1 O4 85.6(4) . 10_556
O2B Co1 O4 84.9(7) . .
O2B Co1 O4 64.3(7) 10_556 .
O1 Co1 O4 157.6(6) 10_556 .
O1 Co1 O4 176.7(5) . .
O2A Co1 O4 85.6(4) 10_556 .
O2A Co1 O4 106.3(4) . .
O4 Co1 O4 20.7(7) 10_556 .
O2B Co1 N2 94.4(5) . 4_556
O2B Co1 N2 94.4(5) 10_556 4_556
O1 Co1 N2 90.1(3) 10_556 4_556
O1 Co1 N2 90.1(3) . 4_556
O2A Co1 N2 86.3(3) 10_556 4_556
O2A Co1 N2 86.3(3) . 4_556
O4 Co1 N2 92.8(5) 10_556 4_556
O4 Co1 N2 92.8(5) . 4_556
O2B Co1 N3 86.0(5) . 5_666
O2B Co1 N3 86.0(5) 10_556 5_666
O1 Co1 N3 88.3(3) 10_556 5_666
O1 Co1 N3 88.3(3) . 5_666
O2A Co1 N3 93.5(3) 10_556 5_666
O2A Co1 N3 93.5(3) . 5_666
O4 Co1 N3 88.9(5) 10_556 5_666
O4 Co1 N3 88.9(5) . 5_666
N2 Co1 N3 178.3(4) 4_556 5_666
O2A Co2 O2A 130.10(13) . 12_655
O2A Co2 O2A 93.9(3) . 2_655
O2A Co2 O2A 64.9(4) 12_655 2_655
O2A Co2 O2A 93.9(3) . 3_665
O2A Co2 O2A 130.10(13) 12_655 3_665
O2A Co2 O2A 93.9(3) 2_655 3_665
O2A Co2 O2A 130.10(13) . 11_665
O2A Co2 O2A 93.9(3) 12_655 11_665
O2A Co2 O2A 130.10(13) 2_655 11_665
O2A Co2 O2A 64.9(4) 3_665 11_665
O2A Co2 O2A 64.9(4) . 10
O2A Co2 O2A 93.9(3) 12_655 10
O2A Co2 O2A 130.10(13) 2_655 10
O2A Co2 O2A 130.10(13) 3_665 10
O2A Co2 O2A 93.9(3) 11_665 10
Co1 O1 Co1 115.9(3) 2_655 3_665
Co1 O1 Co1 115.9(3) 2_655 .
Co1 O1 Co1 115.9(3) 3_665 .
O4 O4 Co1 79.7(3) 10_556 .
C2 C1 C6 117.6(13) . .
C2 C1 P1 125.7(12) . .
C6 C1 P1 116.6(10) . .
C1 C2 C3 123.3(13) . .
C2 C3 C4 117.8(12) . .
C5 C4 C3 119.1(13) . .
C5 C4 N1 122.1(14) . .
C3 C4 N1 118.8(11) . .
C4 C5 C6 123.3(17) . .
C5 C6 C1 118.9(15) . .
N2 C7 N1 113.1(14) . .
N3 C8 N1 111.1(13) . .
C8 N1 C7 103.5(12) . .
C8 N1 C4 127.4(12) . .
C7 N1 C4 129.1(12) . .
C7 N2 N3 105.2(12) . .
C7 N2 Co1 134.9(10) . 4_556
N3 N2 Co1 119.9(8) . 4_556
C8 N3 N2 107.1(12) . .
C8 N3 Co1 131.1(10) . 5_656
N2 N3 Co1 121.8(8) . 5_656
O2B P1 O2B 122.7(14) . 10
O2B P1 O3 83.0(12) . .
O2B P1 O3 99.2(12) 10 .
O2B P1 O3 99.2(12) . 10
O2B P1 O3 83.0(12) 10 10
O3 P1 O3 18.5(18) . 10
O2B P1 O2A 115.2(9) . 10
O2B P1 O2A 30.2(7) 10 10
O3 P1 O2A 129.1(9) . 10
O3 P1 O2A 113.2(9) 10 10
O2B P1 O2A 30.2(7) . .
O2B P1 O2A 115.2(9) 10 .
O3 P1 O2A 113.2(9) . .
O3 P1 O2A 129.1(9) 10 .
O2A P1 O2A 94.5(8) 10 .
O2B P1 C1 117.2(7) . .
O2B P1 C1 117.2(7) 10 .
O3 P1 C1 105.1(8) . .
O3 P1 C1 105.1(8) 10 .
O2A P1 C1 106.5(5) 10 .
O2A P1 C1 106.5(5) . .
O2B O2A P1 66.9(14) . .
O2B O2A Co1 74.3(13) . .
P1 O2A Co1 132.8(6) . .
O2B O2A Co2 146.6(15) . .
P1 O2A Co2 99.1(4) . .
Co1 O2A Co2 127.9(5) . .
O2A O2B P1 82.9(15) . .
O2A O2B Co1 83.1(15) . .
P1 O2B Co1 149.2(12) . .
O3 O3 P1 80.8(9) 10 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2B 2.041(16) .
Co1 O2B 2.041(16) 10_556
Co1 O1 2.100(4) 10_556
Co1 O1 2.100(4) .
Co1 O2A 2.105(8) 10_556
Co1 O2A 2.105(8) .
Co1 O4 2.112(15) 10_556
Co1 O4 2.112(15) .
Co1 N2 2.119(12) 4_556
Co1 N3 2.159(12) 5_666
Co2 O2A 2.190(10) .
Co2 O2A 2.190(10) 12_655
Co2 O2A 2.190(10) 2_655
Co2 O2A 2.190(10) 3_665
Co2 O2A 2.190(10) 11_665
Co2 O2A 2.190(10) 10
O1 Co1 2.100(4) 2_655
O1 Co1 2.100(4) 3_665
O4 O4 0.76(2) 10_556
C1 C2 1.362(19) .
C1 C6 1.43(2) .
C1 P1 1.776(16) .
C2 C3 1.38(2) .
C3 C4 1.42(2) .
C4 C5 1.34(2) .
C4 N1 1.464(17) .
C5 C6 1.36(2) .
C7 N2 1.293(18) .
C7 N1 1.331(17) .
C8 N3 1.310(19) .
C8 N1 1.33(2) .
N2 N3 1.366(16) .
N2 Co1 2.119(12) 4_556
N3 Co1 2.159(12) 5_656
P1 O2B 1.484(16) .
P1 O2B 1.484(16) 10
P1 O3 1.551(18) .
P1 O3 1.552(18) 10
P1 O2A 1.601(9) 10
P1 O2A 1.601(9) .
O2A O2B 0.812(18) .
O3 O3 0.50(5) 10
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.054 951 316 ' '
#BEGIN Loops that were not found in dictionaries:
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 0 1.142
-1 2 0 1.978
#END Loops that were not found in dictionaries
