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_7125852
_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 H37 N7 Ni6 O43 P W9, C6 H20 N4 Ni'
_chemical_formula_sum            'C23 H57 N11 Ni7 O43 P W9'
_chemical_formula_weight         3272.38
_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             2019-08-22
_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                   13.4978(5)
_cell_length_b                   14.1387(5)
_cell_length_c                   35.9568(12)
_cell_measurement_reflns_used    12960
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.2150
_cell_measurement_theta_min      3.0170
_cell_volume                     6862.0(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  52.00   1.00   70.00    --   11.29  19.00-120.00   74
  2  \w     11.00  72.00   1.00   70.00    --  -12.07   0.00 -60.00   61
;
_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      0.0109549000
_diffrn_orient_matrix_UB_12      -0.0488091000
_diffrn_orient_matrix_UB_13      -0.0018842000
_diffrn_orient_matrix_UB_21      0.0401486000
_diffrn_orient_matrix_UB_22      0.0050621000
_diffrn_orient_matrix_UB_23      0.0125838000
_diffrn_orient_matrix_UB_31      -0.0320888000
_diffrn_orient_matrix_UB_32      -0.0103143000
_diffrn_orient_matrix_UB_33      0.0150774000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            25626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    17.004
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38082
_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 dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5972
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.453(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         14632
_refine_ls_number_restraints     1527
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0342P)^2^+12.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13643
_reflns_number_total             14632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09008h2.cif
_cod_data_source_block           n
_cod_depositor_comments
'Adding full bibliography for 7125851--7125854.cif.'
_cod_original_cell_volume        6862.1(4)
_cod_database_code               7125852
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O N P W Ni'
_shelx_estimated_absorpt_t_max   0.727
_shelx_estimated_absorpt_t_min   0.235
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.547(12)
 0.453(12)
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 C(H,H,H,H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C81-C82
 1.5 with sigma of 0.02
 N69-C94B = C94B-C93B = C93B-C95B = C93B-N68
 1.5 with sigma of 0.02
 C95B-N68
 2.3 with sigma of 0.02
 N69-C93A = C93A-C94A = C94A-N68 = C93A-C95A
 1.5 with sigma of 0.02
 N69-C95A
 2.3 with sigma of 0.02
 N71-C90
 1.5 with sigma of 0.02
 C81-C82 = C84-C85 = C90-C92
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N64 \\sim N65 \\sim C81 \\sim C82 \\sim C83: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N66 \\sim N67 \\sim C84 \\sim C85 \\sim C86: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N62 \\sim N63 \\sim C88A \\sim C88B \\sim C87 \\sim C89: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
N70 \\sim N71 \\sim C90 \\sim C91 \\sim C92: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N68 \\sim N69 \\sim C93A \\sim C94B \\sim C93B \\sim C95B \\sim C95A \\sim
C94A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
O47 \\sim O37 \\sim O32 \\sim O43 \\sim O48 \\sim O41 \\sim O21 \\sim O35 \\sim
O18 \\sim O20 \\sim O30 \\sim O26 \\sim O33 \\sim O59 \\sim O52 \\sim O60 \\sim
O22 \\sim O45 \\sim O19 \\sim O31 \\sim O39 \\sim O50 \\sim O29 \\sim O44 \\sim
O40 \\sim O49 \\sim O56 \\sim O55 \\sim O58 \\sim O57 \\sim O46 \\sim O23 \\sim
O28 \\sim O54 \\sim O53 \\sim O36 \\sim O27 \\sim O24 \\sim O42 \\sim O25 \\sim
O34 \\sim O38 \\sim O51: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Ni17 \\sim N71 \\sim N70 \\sim N69 \\sim N68: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C79) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O42) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(H63C)=Sof(H63D)=Sof(H87C)=Sof(H87D)=Sof(H89D)=Sof(H89E)=Sof(H89F)=
 Sof(C88B)=Sof(H88B)=1-FVAR(1)
 Sof(H63A)=Sof(H63B)=Sof(H87A)=Sof(H87B)=Sof(C88A)=Sof(H88A)=Sof(H89A)=
 Sof(H89B)=Sof(H89C)=FVAR(1)
 Sof(H69C)=Sof(H69D)=Sof(H68C)=Sof(H68D)=Sof(C93B)=Sof(H93B)=Sof(C95B)=
 Sof(H95D)=Sof(H95E)=Sof(H95F)=Sof(C94B)=Sof(H94C)=Sof(H94D)=1-FVAR(2)
 Sof(H69A)=Sof(H69B)=Sof(H68A)=Sof(H68B)=Sof(C94A)=Sof(H94A)=Sof(H94B)=
 Sof(C93A)=Sof(H93A)=Sof(C95A)=Sof(H95A)=Sof(H95B)=Sof(H95C)=FVAR(2)
6.a Rotating group:
 O53(H53A,H53B), N72(H72A,H72B)
6.b Ternary CH refined with riding coordinates:
 C90(H90), C82(H82), C85(H85), C88A(H88A), C88B(H88B), C93A(H93A), C93B(H93B)
6.c Secondary CH2 refined with riding coordinates:
 N65(H65A,H65B), N64(H64A,H64B), N66(H66A,H66B), N67(H67A,H67B), N62(H62A,
 H62B), N63(H63A,H63B), N63(H63C,H63D), N69(H69A,H69B), N69(H69C,H69D),
 N70(H70A,H70B), N71(H71A,H71B), N68(H68A,H68B), N68(H68C,H68D), C91(H91A,H91B),
  C81(H81A,H81B), C84(H84A,H84B), C87(H87A,H87B), C87(H87C,H87D), C94A(H94A,
 H94B), C94B(H94C,H94D)
6.d Aromatic/amide H refined with riding coordinates:
 C78(H78), C76(H76), C75(H75)
6.e Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C86(H86A,H86B,H86C), C92(H92A,H92B,H92C), C89(H89A,H89B,
 H89C), C89(H89D,H89E,H89F), C95A(H95A,H95B,H95C), C95B(H95D,H95E,H95F)
;
_shelx_res_checksum              53935
_shelx_fab_checksum              64807
_olex2_date_sample_data_collection 2019-07-18
_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 1.997
_oxdiff_exptl_absorpt_empirical_full_min 0.695