A bi-polyoxometallate-based host-guest metal-organic framework.
Wang, Sa-Sa; Yang, Wen-Bin; Yang, Mingxue; Wu, Xiao-Yuan; Wu, Weiming; Wang, Song-Xia; Lin, Lang; Lu, Can-Zhong; Chemical communications (Cambridge, England) 56 (2020) 2503–2506; doi:10.1039/c9cc09008h

data_7125853
_publ_section_title
;
 A bi-polyoxometallate-based host-guest metal-organic framework.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2503
_journal_page_last               2506
_journal_paper_doi               10.1039/c9cc09008h
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H38 N6 Ni6 O43 P W9, C6 H20 N4 Ni, H2 O'
_chemical_formula_sum            'C23 H58 N10 Ni7 O43 P W9'
_chemical_formula_weight         3259.38
_chemical_name_systematic        orthorhombic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-22 deposited with the CCDC.	2020-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4578(4)
_cell_length_b                   14.1507(6)
_cell_length_c                   36.0116(11)
_cell_measurement_reflns_used    22544
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.0400
_cell_measurement_theta_min      3.4570
_cell_volume                     6858.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  89.00   0.60    8.25    --   11.43  77.00-180.00  185
  2  \w     73.00 100.00   0.60    8.25    --   11.43 178.00-150.00   45
  3  \w    -11.00  57.40   0.60    8.25    --   11.43  19.00 150.00  114
  4  \w    -23.00   4.00   0.60    8.25    --   11.43 -38.00   0.00   45
  5  \w    -31.00  43.40   0.60    8.25    --   11.43 -77.00  30.00  124
  6  \w    -81.00  -9.00   0.60    8.25    --  -12.22 -57.00 -90.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0371005000
_diffrn_orient_matrix_UB_12      0.0350206000
_diffrn_orient_matrix_UB_13      0.0025872000
_diffrn_orient_matrix_UB_21      -0.0267155000
_diffrn_orient_matrix_UB_22      0.0311057000
_diffrn_orient_matrix_UB_23      -0.0117064000
_diffrn_orient_matrix_UB_31      -0.0262469000
_diffrn_orient_matrix_UB_32      0.0178108000
_diffrn_orient_matrix_UB_33      0.0155941000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            62795
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    17.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5948
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.244
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.479(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         15049
_refine_ls_number_restraints     705
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0376
_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/[\s^2^(Fo^2^)+(0.0295P)^2^+42.6613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13681
_reflns_number_total             15049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09008h2.cif
_cod_data_source_block           hchain
_cod_depositor_comments
'Adding full bibliography for 7125851--7125854.cif.'
_cod_database_code               7125853
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C N O H P W Ni'
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.132
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.521(11)
 0.479(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H)
  groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C89B-N23
 1.5 with sigma of 0.02
 C89B-C88
 1.5 with sigma of 0.02
 C90A-C89B
 1.5 with sigma of 0.02
 C91A-C92A
 1.5 with sigma of 0.02
 C93A-C92A
 1.5 with sigma of 0.02
 C93A-C91A
 2.3 with sigma of 0.02
 C92B-C91B
 1.5 with sigma of 0.02
 C93B-C92B
 1.5 with sigma of 0.02
 C93B-C91B
 2.3 with sigma of 0.02
 C83-C82
 1.5 with sigma of 0.02
 C83-C84
 1.5 with sigma of 0.02
 C79-C80
 1.5 with sigma of 0.02
 C88-N24
 1.5 with sigma of 0.02
 N22-C83 = C83-C82 = C83-C84
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C90A \\sim C89A \\sim N23: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C72 \\sim C71 \\sim C73 \\sim C82 \\sim C84 \\sim C83 \\sim C79 \\sim C86A
\\sim C75 \\sim C77 \\sim C74 \\sim C81 \\sim C80 \\sim C78 \\sim C76 \\sim
C90A \\sim C88 \\sim C89B \\sim C90B \\sim C89A \\sim C86B \\sim C85B \\sim
C85A \\sim C91A \\sim C92A \\sim C93A \\sim C92B \\sim C93B \\sim C91B \\sim
C87A \\sim C87B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C82 \\sim N21 \\sim C83: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Ni7 \\sim N25 \\sim N26 \\sim N23 \\sim N24: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Ni16 \\sim N21 \\sim N22 \\sim O53 \\sim O65 \\sim O62 \\sim O68: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O61) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O56)
\\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O50) \\sim Ueq,
Uanis(O62) \\sim Ueq, Uanis(O67) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C85A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O53) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C86B) \\sim Ueq, Uanis(C85B) \\sim Ueq, Uanis(N20) \\sim Ueq, Uanis(C90B)
\\sim Ueq, Uanis(C89A) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C73) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C92A) \\sim Ueq, Uanis(C93A) \\sim Ueq, Uanis(C91B)
\\sim Ueq, Uanis(C92B) \\sim Ueq, Uanis(C91A) \\sim Ueq, Uanis(C93B) \\sim Ueq,
Uanis(C83) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C86A) \\sim Ueq, Uanis(C86A) \\sim Ueq, Uanis(C90A) \\sim Ueq,
Uanis(C89B) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C87A)
\\sim Ueq, Uanis(C87B) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
5. Rigid body (RIGU) restrains
 N22, N21, C82, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N18, N17, C79, C80, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H20C)=Sof(H20D)=Sof(H23C)=Sof(H23D)=Sof(H19C)=Sof(H19D)=Sof(H88C)=
 Sof(H88D)=Sof(C90B)=Sof(H90D)=Sof(H90E)=Sof(H90F)=Sof(C89A)=Sof(H89A)=
 Sof(C86B)=Sof(H86B)=Sof(C85B)=Sof(H85A)=Sof(H85B)=Sof(C87B)=Sof(H87D)=
 Sof(H87E)=Sof(H87F)=1-FVAR(1)
 Sof(H20A)=Sof(H20B)=Sof(H23A)=Sof(H23B)=Sof(H19A)=Sof(H19B)=Sof(C86A)=
 Sof(H86A)=Sof(C90A)=Sof(H90A)=Sof(H90B)=Sof(H90C)=Sof(H88A)=Sof(H88B)=
 Sof(C89B)=Sof(H89B)=Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C87A)=Sof(H87A)=
 Sof(H87B)=Sof(H87C)=FVAR(1)
 Sof(H26C)=Sof(H26D)=Sof(H25C)=Sof(H25D)=Sof(C92B)=Sof(H92B)=Sof(C93B)=
 Sof(H93D)=Sof(H93E)=Sof(H93F)=Sof(C91B)=Sof(H91C)=Sof(H91D)=1-FVAR(2)
 Sof(H26A)=Sof(H26B)=Sof(H25A)=Sof(H25B)=Sof(C91A)=Sof(H91A)=Sof(H91B)=
 Sof(C92A)=Sof(H92A)=Sof(C93A)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(2)
7.a Free rotating group:
 O1(H1A,H1B)
7.b Rotating group:
 O59(H59A,H59B), O55(H55A,H55B)
7.c Ternary CH refined with riding coordinates:
 C83(H83), C86A(H86A), C80(H80), C89B(H89B), C89A(H89A), C86B(H86B),
 C92A(H92A), C92B(H92B)
7.d Secondary CH2 refined with riding coordinates:
 N22(H22A,H22B), N21(H21A,H21B), N17(H17A,H17B), N20(H20C,H20D), N20(H20A,
 H20B), N18(H18A,H18B), N23(H23A,H23B), N23(H23C,H23D), N24(H24A,H24B),
 N19(H19A,H19B), N19(H19C,H19D), N26(H26A,H26B), N26(H26C,H26D), C82(H82A,H82B),
  N25(H25A,H25B), N25(H25C,H25D), C79(H79A,H79B), C88(H88A,H88B), C88(H88C,
 H88D), C85B(H85A,H85B), C85A(H85C,H85D), C91A(H91A,H91B), C91B(H91C,H91D)
7.e Aromatic/amide H refined with riding coordinates:
 C73(H73), C75(H75), C77(H77), C74(H74)
7.f Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C81(H81A,H81B,H81C), C90A(H90A,H90B,H90C), C90B(H90D,
 H90E,H90F), C93A(H93A,H93B,H93C), C93B(H93D,H93E,H93F), C87A(H87A,H87B,H87C),
 C87B(H87D,H87E,H87F)
;
_shelx_res_checksum              66156
_shelx_fab_checksum              95571
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.466
_oxdiff_exptl_absorpt_empirical_full_min 0.646