Syntheses, structures and catalytic properties of Evans-Showell-type polyoxometalate-based 3D metal-organic complexes constructed from the semi-rigid bis(pyridylformyl)piperazine ligand and transition metals.
Li, Feng-Cai; Tan, Li-Kun; Li, Xi-Li; Kong, Hua-Jie; Ge, Li-Ming; Yue, Ling-Yu; Han, Li-Feng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5831–5841; doi:10.1039/c9dt00499h

data_7049550
_publ_section_title
;
 Syntheses, structures and catalytic properties of Evans-Showell-type
 polyoxometalate-based 3D metal-organic complexes constructed from the
 semi-rigid bis(pyridylformyl)piperazine ligand and transition metals.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5831
_journal_page_last               5841
_journal_paper_doi               10.1039/c9dt00499h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'0.5(C32 H56 Co4 Mo20 N8 O96 Zn4), C16 H16 N4 O2'
_chemical_formula_sum            'C32 H44 Co2 Mo10 N8 O50 Zn2'
_chemical_formula_weight         2548.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-14 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.817(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.544(2)
_cell_length_b                   14.2328(12)
_cell_length_c                   24.246(3)
_cell_measurement_reflns_used    8085
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      29.3350
_cell_measurement_theta_min      4.0170
_cell_volume                     7187.4(13)
_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      298.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17793
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         3.648
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46922
_exptl_absorpt_correction_type   multi-scan
_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    2.355
_exptl_crystal_description       block
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.009
_refine_diff_density_min         -2.305
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0921
_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^)+(0.0456P)^2^+642.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             7033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00499h2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7049549--7049550.cif.'
_cod_original_cell_volume        7187.6(12)
_cod_database_code               7049550
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
 O22(H22A,H22B), O23(H23A,H23B), O24(H24A,H24B)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'