Crystal structure of bis(2,5,5,7-tetramethyl-1,4-diazepane-1,4-diium) diaqua-bis(1,2-diaminopropane)copper(II) bis(μ6-oxido)tetrakis(μ3-oxido)-tetradecakis(μ2-oxido)-octaoxido-decavanadium(V) – water (1/4), C24H76CuN8V10O34
Deng, Yuan-Huan; Wang, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 345–347; doi:10.1515/ncrs-2022-0542

data_8107436
_publ_section_title
;
 Crystal structure of bis(2,5,5,7-tetramethyl-1,4-diazepane-1,4-diium)
 diaqua-bis(1,2-diaminopropane)copper(II)
 bis(\m6-oxido)tetrakis(\m3-oxido)-tetradecakis(\m2-oxido)-octaoxido-decavanadium(V)
 -- water (1/4), C24H76CuN8V10O34
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              345
_journal_page_last               347
_journal_paper_doi               10.1515/ncrs-2022-0542
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'O28 V10, C6 H20 Cu N4, 2(C9 H22 N2), 6(H2 O)'
_chemical_formula_sum            'C24 H76 Cu N8 O34 V10'
_chemical_formula_weight         1593.86
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.594(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.416(4)
_cell_length_b                   11.7003(18)
_cell_length_c                   20.079(3)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.25
_cell_volume                     5241.1(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II'
_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  0.0170
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.701
_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    2.195
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_correction_T_min  0.5401
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3228
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.72
_exptl_transmission_factor_min   0.54
_refine_diff_density_max         1.130
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.504
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6030
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+2.4105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5457
_reflns_number_total             6030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0542_suppl.cif
_cod_data_source_block           0
_cod_original_cell_volume        5241.2(14)
_cod_database_code               8107436
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.540
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1WA-H1WB = H2WB-H2WA = H3WB-H3WA
 1.39 with sigma of 0.01
 O1W-H1WA = O1W-H1WB = O2W-H2WB = O2W-H2WA
 0.86 with sigma of 0.01
 O3W-H3WB = O3W-H3WA
 0.86 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N2(H2A,H2B), C9(H9A,H9B), N1(H1A,H1B), C4(H4C,H4D),
 C1(H1C,H1D)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C),
 C3(H3C,H3D,H3E)
;
_shelx_res_checksum              99113
_shelx_hkl_checksum              72181
_olex2_submission_special_instructions 'No special instructions were received'