Crystal structure of catena-poly[bis(4,4′-dipyridylaminium-kN)-(μ2-germanowolframato-κ2 O:O′)-(2,2′-bipyridine-κ2 N,N′)copper(II)] with a Keggin-type heteropolyoxoanion, [Cu(C10H8N2)(C10H10N3)2][GeW12O40] ⋅ H2O
Wu, Li-Zhou; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1007–1010; doi:10.1515/ncrs-2018-0132

data_8106379
_publ_section_title
;
 Crystal structure of
 catena-poly[bis(4,4&#x2032;-dipyridylaminium-kN)-(\m2-germanowolframato-\k2
 O:O&#x2032;)-(2,2&#x2032;-bipyridine-\k2 N,N&#x2032;)copper(II)] with a
 Keggin-type heteropolyoxoanion, [Cu(C10H8N2)(C10H10N3)2][GeW12O40]
 &#x22C5; H2O
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1007
_journal_page_last               1010
_journal_paper_doi               10.1515/ncrs-2018-0132
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C30 H28 Cu Ge N8 O40 W12, H2 O'
_chemical_formula_sum            'C30 H30 Cu Ge N8 O41 W12'
_chemical_formula_weight         3500.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90.221(3)
_cell_angle_beta                 92.188(3)
_cell_angle_gamma                108.966(3)
_cell_formula_units_Z            2
_cell_length_a                   12.095(2)
_cell_length_b                   13.488(3)
_cell_length_c                   19.220(4)
_cell_measurement_reflns_used    3632
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.26
_cell_volume                     2962.7(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.1029
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16457
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.910
_diffrn_reflns_theta_min         1.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.140
_exptl_absorpt_correction_T_max  0.310
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.924
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3086
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.388
_refine_diff_density_min         -5.722
_refine_diff_density_rms         0.602
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         11935
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8794
_reflns_number_total             11935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0132_suppl.cif
_cod_data_source_block           xb6933_0m
_cod_original_cell_volume        2962.8(10)
_cod_database_code               8106379
_shelx_estimated_absorpt_t_max   0.220
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H29-H24
 2.2 with sigma of 0.02
3. Rigid bond restraints
 N5, N7, C2, C3, C20, C23, C26, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O14) \\sim
Ueq, Uanis(O15) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O27) \\sim Ueq,
Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(N1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O23) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
6.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30)
;
_olex2_submission_special_instructions 'No special instructions were received'