Four Hybrid Materials Based on Preyssler P5W30 Polyoxometalate and First-Row Transition-Metal Complex.
Hu, Tuo-Ping; Zhao, Ya-Qin; Jagličić, Zvonko; Yu, Kai; Wang, Xing-Po; Sun, Di; Inorganic chemistry 54 (2015) 7415–7423; doi:10.1021/acs.inorgchem.5b00962

data_4343998
_publ_section_title
;
 Four Hybrid Materials Based on Preyssler P5W30 Polyoxometalate and
 First-Row Transition-Metal Complex.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7415
_journal_page_last               7423
_journal_paper_doi               10.1021/acs.inorgchem.5b00962
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C60 H84 Co4 K N24 O120 P5 W30'
_chemical_formula_sum            'C60 H84 Co4 K N24 O120 P5 W30'
_chemical_formula_weight         9005.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.019(2)
_cell_length_b                   38.427(3)
_cell_length_c                   38.738(3)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.297
_cell_measurement_theta_min      2.366
_cell_volume                     40220(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SAINT'
_computing_publication_material  'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1326
_diffrn_reflns_av_unetI/netI     0.2176
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            160047
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.826
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    17.549
_exptl_absorpt_correction_T_max  0.3341
_exptl_absorpt_correction_T_min  0.2272
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.975
_exptl_crystal_description       plate
_exptl_crystal_F_000             31944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.984
_refine_diff_density_min         -2.148
_refine_diff_density_rms         0.571
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2196
_refine_ls_number_reflns         32173
_refine_ls_number_restraints     596
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.1146
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1065P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17940
_reflns_number_total             32173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00962_si_002.cif
_cod_data_source_block           p4
_cod_depositor_comments
'Adding full bibliography for 4343995--4343998.cif.'
_cod_database_code               4343998
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C45
 1.55 with sigma of 0.01
 C26-C27
 1.55 with sigma of 0.01
 C56-C57
 1.55 with sigma of 0.01
 O1WA-K1A
 1 with sigma of 0.01
3. Restrained planarity
 C5, N2, C2, C1, N1, C3, C4
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
N4 \\sim N3: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
N11: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.08
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim N10 \\sim N9 \\sim C28:
within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.08
C12 \\sim C13 \\sim C14 \\sim C27 \\sim C29 \\sim C4 \\sim C34 \\sim C46 \\sim
C60 \\sim C33 \\sim C3 \\sim C31 \\sim C9 \\sim C39 \\sim C36 \\sim C2 \\sim
C40 \\sim C35 \\sim C32 \\sim C42 \\sim C49 \\sim C48 \\sim C50 \\sim C41 \\sim
C37 \\sim C38 \\sim C28 \\sim C30 \\sim C54 \\sim C51 \\sim C44 \\sim C45 \\sim
C47 \\sim C43 \\sim C26 \\sim C52 \\sim C55 \\sim C59 \\sim C57 \\sim C58 \\sim
C53 \\sim C8 \\sim C15 \\sim C6 \\sim C11 \\sim C10 \\sim C7 \\sim C5 \\sim C1
\\sim C56 \\sim C16 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim N1 \\sim N2
\\sim N24 \\sim N23 \\sim N7 \\sim N8 \\sim N11 \\sim N12: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
K1 \\sim K1A \\sim O1W \\sim O1WA: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.08
Uanis(O77) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O63)
\\sim Ueq, Uanis(O83) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(O96) \\sim Ueq,
Uanis(O97) \\sim Ueq, Uanis(O92) \\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O44) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O87) \\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O110)
\\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(O47) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1W) \\sim Ueq, Uanis(O1WA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.2
Uanis(K1) \\sim Ueq, Uanis(K1A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: K1(0.35) K1A(0.65) O1W(0.5) O1WA(0.5)
6.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C56(H56A,H56B,H56C)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N11(H11), N14(H14), N16(H16), N17(H17), N20(H20), N21(H21),
 N7(H7), N9(H9), N24(H24)
6.c Fitted pentagon refined as free rotating group:
 N5(N6,C12,C13,C14), C19(C18,C17,N8,N7), C23(C24,N10,N9,C22), C59(N23,N24,C57,
 C58)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C55(H55A,H55B,H55C), C60(H60A,H60B,H60C)
;