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_7125851
_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_formula_moiety
'2(H2 Na Ni0.99 O41 P W11.01), C84 H138 N24 Ni24 O190 P4 S6 W36, 2(C12 H40 N8 Ni2), 4(C6 H24 N4 Ni O2), 4(C5.5 H19.5 N4 Ni)'
_chemical_formula_sum            'C154 H396 N72 Na2 Ni37.99 O280 P6 S6 W58.01'
_chemical_formula_weight         21056.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-11 deposited with the CCDC.	2020-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.026(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.311(3)
_cell_length_b                   39.040(4)
_cell_length_c                   27.663(5)
_cell_measurement_reflns_used    9351
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.29
_cell_volume                     24197(6)
_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_temperature      200.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            177017
_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         25.500
_diffrn_reflns_theta_min         2.223
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.302
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             19250
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.027
_refine_diff_density_max         4.560
_refine_diff_density_min         -3.654
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1494
_refine_ls_number_reflns         22879
_refine_ls_number_restraints     570
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+805.4865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16904
_reflns_number_total             22879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09008h2.cif
_cod_data_source_block           wss0412_0m-15a
_cod_depositor_comments
'Adding full bibliography for 7125851--7125854.cif.'
_cod_database_code               7125851
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N8-N75
 2.8 with sigma of 0.02
 Ni7-C48_$1
 2.8 with sigma of 0.02
 Ni7-C49_$1
 2.8 with sigma of 0.02
 Ni7-C46_$1
 2.8 with sigma of 0.02
 Ni7-C45_$1
 2.8 with sigma of 0.02
 N74-N7
 2.8 with sigma of 0.02
 N74-C46 = C45-C46 = N7-C45 = N75-C48 = C49-C48 = N8-C49
 1.48 with sigma of 0.01
 Ni7-N7_$1 = Ni7-N74_$1 = Ni7-N75_$1 = Ni7-N8_$1
 2 with sigma of 0.02
 C36-C35 = N17-C35 = N18-C36
 1.48 with sigma of 0.02
 N19-C39 = C39-C38 = N20-C38
 1.48 with sigma of 0.02
 Ni10-N19_$1 = Ni10-N20_$1 = Ni10-N18_$1 = Ni10-N17_$1
 1.85 with sigma of 0.02
 Ni10-C39_$1 = Ni10-C35_$1
 2.8 with sigma of 0.02
 N17-N18
 2.8 with sigma of 0.02
 N20-N19
 2.8 with sigma of 0.02
 N19-C39 = C39-C38 = N20-C38 = N18-C36 = N17-C35 = C36-C35
 1.48 with sigma of 0.02
 Ni10-C36_$1
 2.8 with sigma of 0.02
 Ni10-C38_$1
 2.8 with sigma of 0.02
 N15-C29 = C30-C29 = N16-C30 = C31-C30
 1.5 with sigma of 0.01
 C34-C33 = C33-C32 = N13-C32 = N14-C33
 1.5 with sigma of 0.01
 C49-C50 = C46-C47
 1.48 with sigma of 0.01
 C48-C50 = C45-C47
 2.5 with sigma of 0.02
 C45-C47 = C47-N74
 2.6 with sigma of 0.02
 C37-C35 = C40-C39
 1.48 with sigma of 0.01
 C40-N19
 2.5 with sigma of 0.02
 C38-C40
 2.5 with sigma of 0.02
 N17-C37
 2.5 with sigma of 0.02
 C37-C36
 2.5 with sigma of 0.02
 C36-C37 = C37-N17
 2.6 with sigma of 0.02
 Na1-O25A = Na1-O25
 1.9 with sigma of 0.01
3. Restrained planarity
 Ni7, N7_$1, N8_$1, N74_$1, N75_$1
 with sigma of 0.01
 Ni10, N17_$1, N18_$1, N19_$1, N20_$1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N7 \\sim N8 \\sim N74 \\sim N75 \\sim C50 \\sim C47 \\sim C46 \\sim C45 \\sim
C48 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N19 \\sim N20 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N5 \\sim N6 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Ni2A \\sim W2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N74) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(N75) \\sim Ueq, Uanis(N8) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(N19) \\sim Ueq, Uanis(N20)
\\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O25A) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(W2) \\sim Ueq, Uanis(Ni2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N18) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(N17) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N13) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(N14)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(N16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O25A) = Uanis(O25)
Uanis(Ni1A) = Uanis(W1)
Uanis(Ni2A) = Uanis(W2)
Uanis(Ni7) = Uanis(N8) = Uanis(N7) = Uanis(N74) = Uanis(N75)
5. Rigid body (RIGU) restrains
 N7, N8, N74, N75, C50, C47, C46, C45, C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N19, N20, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, N6, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N17, C35, C37, C36, N18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, C33, C32, N13, N14, N15, C29, C30, C31, N16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(O25A)=Sof(H25F)=Sof(H25G)=0.5*(1-FVAR(2))
 Sof(O25)=Sof(H25D)=Sof(H25E)=0.5*FVAR(2)
 Sof(Ni2A)=1-FVAR(2)
 Sof(W2)=FVAR(2)
 Sof(Ni1A)=0.5*(1-FVAR(4))
 Sof(W1)=0.5*FVAR(4)
 Fixed Sof: N7(0.5) H7A(0.5) H7B(0.5) N8(0.5) H8A(0.5) H8B(0.5) N74(0.5)
 H74A(0.5) H74B(0.5) N75(0.5) H75A(0.5) H75B(0.5) C50(0.5) H50A(0.5) H50B(0.5)
 H50C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C46(0.5) H46(0.5) C45(0.5)
 H45A(0.5) H45B(0.5) C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49(0.5) C33(0.5)
 H33(0.5) N17(0.5) H17C(0.5) H17D(0.5) N18(0.5) H18A(0.5) H18B(0.5) N19(0.5)
 H19D(0.5) H19E(0.5) N20(0.5) H20C(0.5) H20D(0.5) C35(0.5) H35(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) C39(0.5) H39(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
 Fixed U11: C48(0.206372)
 Fixed U12: C48(-0.000134)
 Fixed U13: C48(0.00134)
 Fixed U22: C48(0.20968)
 Fixed U23: C48(-0.0008)
 Fixed U33: C48(0.20843)
7.a Riding coordinates:
 O25(H25D,H25E), C25(H25A,H25B,H25C), O76(H76A,H76B), O77(H77A,H77B),
 O25A(H25F,H25G)
7.b Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C24(H24), C46(H46), C49(H49), C21(H21), C27(H27),
 C30(H30), C33(H33), C35(H35), C39(H39)
7.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 C14(H14A,H14B), C17(H17A,H17B), C23(H23A,H23B), N7(H7A,H7B), N8(H8A,H8B),
 N74(H74A,H74B), N75(H75A,H75B), C45(H45A,H45B), C48(H48A,H48B), N9(H9A,H9B),
 N10(H10A,H10B), N11(H11A,H11B), N12(H12A,H12B), C20(H20A,H20B), C26(H26A,H26B),
  N13(H13A,H13B), N14(H14C,H14D), N15(H15A,H15B), N16(H16D,H16E), C29(H29A,
 H29B), C32(H32A,H32B), N17(H17C,H17D), N18(H18A,H18B), N19(H19D,H19E),
 N20(H20C,H20D), C36(H36A,H36B), C38(H38A,H38B)
7.d Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C50(H50A,H50B,H50C), C47(H47A,H47B,
 H47C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C34(H34A,
 H34B,H34C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C)
7.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12)
;
_shelx_res_checksum              15032
_shelx_fab_checksum              18773
_olex2_submission_special_instructions 'No special instructions were received'