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_7049549
_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
'C16 H26 Co2 Cu2 Mo10 N4 O45, C16 H22 Cu N4 O5'
_chemical_formula_sum            'C32 H48 Co2 Cu3 Mo10 N8 O50'
_chemical_formula_weight         2612.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                78.079(4)
_cell_angle_beta                 82.282(4)
_cell_angle_gamma                83.825(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1598(5)
_cell_length_b                   14.1021(6)
_cell_length_c                   23.8608(12)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3700
_cell_measurement_theta_min      3.3380
_cell_volume                     3953.6(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37927
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         3.008
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70871
_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    2.195
_exptl_crystal_description       block
_exptl_crystal_F_000             2514
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.606
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         16348
_refine_ls_number_restraints     1020
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0923
_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^)+(0.0871P)^2^+116.2981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11050
_reflns_number_total             16348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00499h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7049549--7049550.cif.'
_cod_database_code               7049549
_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
O1 \\sim O50 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16
\\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24
\\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32
\\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40
\\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O41 \\sim O42 \\sim O47 \\sim O48
\\sim O49: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
 O50(H50a,H50b), O43(H43a,H43b), O44(H44a,H44b), O45(H45a,H45b), O46(H46a,
 H46b), O47(Hp,Hq), O48(Hr,Hs), O49(Ht,Hu)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C15(H15a,H15b), C16(H16a,H16b), C23(Hd,He), C24(Hf,
 Hg), C25(Hh,Hi), C26(Hj,Hk)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C17(H),
 C18(Ha), C19(Hb), C20(Hc), C29(Hl), C30(Hm), C31(Hn), C32(Ho)
;
_olex2_submission_special_instructions 'No special instructions were received'