Evans-Showell-type polyoxometalate-based metal-organic complexes with novel 3D structures constructed from flexible bis-pyrazine-bis-amide ligands and copper metals: syntheses, structures, and fluorescence and catalytic properties.
Li, Feng-Cai; Li, Xi-Li; Tan, Li-Kun; Wang, Jin-Tang; Yao, Wei-Zhong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2160–2169; doi:10.1039/c8dt04698k

data_7048621
_publ_section_title
;
 Evans-Showell-type polyoxometalate-based metal-organic complexes with
 novel 3D structures constructed from flexible bis-pyrazine-bis-amide
 ligands and copper metals: syntheses, structures, and fluorescence and
 catalytic properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2160
_journal_page_last               2169
_journal_paper_doi               10.1039/c8dt04698k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C21 H24 Co2 Cu3 Mo10 N9 O46, H2 O'
_chemical_formula_sum            'C21 H26 Co2 Cu3 Mo10 N9 O47'
_chemical_formula_weight         2424.39
_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             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2019-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                76.352(4)
_cell_angle_beta                 71.082(4)
_cell_angle_gamma                89.701(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4355(5)
_cell_length_b                   15.6728(8)
_cell_length_c                   17.6863(9)
_cell_measurement_reflns_used    9518
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.1520
_cell_measurement_theta_min      3.4990
_cell_volume                     3159.2(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
_diffrn_measured_fraction_theta_full 0.998
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28988
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    3.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82923
_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    2.549
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.072
_refine_diff_density_min         -2.172
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13046
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0584P)^2^+11.9984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9740
_reflns_number_total             13046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04698k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048621--7048622.cif.'
_cod_database_code               7048621
_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, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C20(H20A,H20B), C21(H21A,
 H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), N3(H3A), N4(H4), N9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'