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_7125854
_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 O44 P W9, C6 H20 N4 Ni, H2 O'
_chemical_formula_sum            'C23 H60 N10 Ni7 O45 P W9'
_chemical_formula_weight         3293.40
_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     iterative
_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                   13.5091(2)
_cell_length_b                   14.2789(2)
_cell_length_c                   36.1110(6)
_cell_measurement_reflns_used    26564
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      30.7460
_cell_measurement_theta_min      3.6250
_cell_volume                     6965.63(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -18.00   94.00   0.5000    8.6750
omega____ theta____ kappa____ phi______ frames
    -       15.4102   77.0000   90.0000 224

  2 omega   11.00   92.00   0.5000    8.6750
omega____ theta____ kappa____ phi______ frames
    -       15.4102   77.0000 -150.0000 162

  3 omega   27.00   59.00   0.5000    8.6750
omega____ theta____ kappa____ phi______ frames
    -      -15.5664   77.0000  -60.0000 64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0188406000
_diffrn_orient_matrix_UB_12      0.0455135000
_diffrn_orient_matrix_UB_13      0.0034958000
_diffrn_orient_matrix_UB_21      0.0325282000
_diffrn_orient_matrix_UB_22      -0.0187062000
_diffrn_orient_matrix_UB_23      0.0135445000
_diffrn_orient_matrix_UB_31      0.0366381000
_diffrn_orient_matrix_UB_32      -0.0067669000
_diffrn_orient_matrix_UB_33      -0.0137984000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            40345
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6020
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.404
_refine_diff_density_min         -2.606
_refine_diff_density_rms         0.312
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.036(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         16970
_refine_ls_number_restraints     549
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+36.3214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                16382
_reflns_number_total             16970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09008h2.cif
_cod_data_source_block           exp_30008
_cod_depositor_comments
'Adding full bibliography for 7125851--7125854.cif.'
_cod_original_cell_volume        6965.63(19)
_cod_database_code               7125854
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ni W C O N P H'
_shelx_estimated_absorpt_t_max   0.285
_shelx_estimated_absorpt_t_min   0.113
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.964(10)
 0.036(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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 C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
3. Restrained distances
 H59A-H1WB
 2.3 with sigma of 0.01
 H59A-H1WA
 2.3 with sigma of 0.01
 C80-C79
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C88 \\sim C78 \\sim C72 \\sim C75 \\sim C73 \\sim C77 \\sim C74 \\sim C76 \\sim
C93 \\sim C89 \\sim C94 \\sim C92 \\sim C90 \\sim C91 \\sim C82A \\sim C83A
\\sim C83B \\sim C84 \\sim C85A \\sim C86A \\sim C82B \\sim C81 \\sim C87 \\sim
C86B \\sim C85B \\sim C79 \\sim C80: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N66 \\sim C80 \\sim C79 \\sim C81 \\sim N67: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C89 \\sim C90 \\sim C91 \\sim N69 \\sim N68: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C93 \\sim N71 \\sim C92 \\sim C94 \\sim N70: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O57) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C83A) \\sim Ueq, Uanis(C83B)
\\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(C85B) \\sim Ueq, Uanis(C82A) \\sim Ueq,
Uanis(C82B) \\sim Ueq, Uanis(C86B) \\sim Ueq, Uanis(C86A) \\sim Ueq, Uanis(O40)
\\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(N65) \\sim Ueq,
Uanis(O41) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C85A)
\\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(O42)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(H64C)=Sof(H64D)=Sof(H65C)=Sof(H65D)=Sof(H63C)=Sof(H63D)=Sof(H62C)=
 Sof(H62D)=Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(C83A)=Sof(H83A)=Sof(H84D)=
 Sof(H84E)=Sof(H84F)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(C86B)=Sof(H86B)=
 Sof(C85B)=Sof(H85C)=Sof(H85D)=1-FVAR(1)
 Sof(H64A)=Sof(H64B)=Sof(H65A)=Sof(H65B)=Sof(H63A)=Sof(H63B)=Sof(H62A)=
 Sof(H62B)=Sof(C83B)=Sof(H83B)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C85A)=
 Sof(H85A)=Sof(H85B)=Sof(C86A)=Sof(H86A)=Sof(C82B)=Sof(H82C)=Sof(H82D)=
 Sof(H87A)=Sof(H87B)=Sof(H87C)=FVAR(1)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Rotating group:
 O59(H59A,H59B), O53(H53A,H53B)
6.c Ternary CH refined with riding coordinates:
 C92(H92), C90(H90), C83A(H83A), C83B(H83B), C86A(H86A), C86B(H86B), C80(H80)
6.d Secondary CH2 refined with riding coordinates:
 N64(H64C,H64D), N64(H64A,H64B), N65(H65C,H65D), N65(H65A,H65B), N67(H67A,
 H67B), N63(H63A,H63B), N63(H63C,H63D), N66(H66A,H66B), N69(H69A,H69B),
 N62(H62A,H62B), N62(H62C,H62D), N71(H71A,H71B), N70(H70A,H70B), C93(H93A,H93B),
  C89(H89A,H89B), N68(H68A,H68B), C82A(H82A,H82B), C85A(H85A,H85B), C82B(H82C,
 H82D), C85B(H85C,H85D), C79(H79A,H79B)
6.e Aromatic/amide H refined with riding coordinates:
 C78(H78), C74(H74), C76(H76)
6.f Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C91(H91A,H91B,H91C), C84(H84D,H84E,H84F), C84(H84A,H84B,
 H84C), C81(H81A,H81B,H81C), C87(H87A,H87B,H87C), C87(H87D,H87E,H87F)
6.g Idealised tetrahedral OH refined as rotating group:
 O61(H61)
;
_shelx_res_checksum              64676
_shelx_fab_checksum              5473
_olex2_submission_special_instructions 'No special instructions were received'