Copper(II)‒ethylenediamine linked Nb24 dimer with one dimensional chain architecture
Li, Nan; Wei, Genlong; Cheng, Mengyuan; Pang, Xiaoshuai; Wang, Ke; Wang, Guan; Zhang, Dongdi; Inorganica Chimica Acta 508 (2020) 119646–; doi:10.1016/j.ica.2020.119646

data_1564594
_publ_section_title
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 Copper(II)--ethylenediamine linked Nb24 dimer with one dimensional chain
 architecture
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_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119646
_journal_paper_doi               10.1016/j.ica.2020.119646
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety
'2(C4 Cu N4 Nb24 O72), 2(C4 Cu N4 O), 4(C4 Cu N4), 74(O), 6(C2 N2)'
_chemical_formula_sum            'C44 Cu8 N44 Nb48 O220'
_chemical_formula_weight         9632.88
_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   .
_atom_sites_solution_primary     iterative
_cell_angle_alpha                94.957(7)
_cell_angle_beta                 102.512(8)
_cell_angle_gamma                110.026(7)
_cell_formula_units_Z            1
_cell_length_a                   16.945(10)
_cell_length_b                   17.795(11)
_cell_length_c                   26.030(15)
_cell_measurement_reflns_used    9104
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.35
_cell_volume                     7088(7)
_computing_cell_refinement       si2w18co4
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        si2w18co4
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41387
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         0.814
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1111 before and 0.0365 after correction.
The Ratio of minimum to maximum transmission is 0.6359.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_description       block
_exptl_crystal_F_000             4532
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.4742
_refine_diff_density_max         2.823
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1651
_refine_ls_number_reflns         28490
_refine_ls_number_restraints     2338
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0769P)^2^+38.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                23965
_reflns_number_total             28490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-508-119646.cif
_cod_data_source_block           P-1_a
_cod_database_code               1564594
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
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1. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O67) \\sim Ueq, Uanis(O76)
\\sim Ueq, Uanis(O77) \\sim Ueq, Uanis(O93) \\sim Ueq, Uanis(O94) \\sim Ueq,
Uanis(O95) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O88) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O91(0.5) O102(0.5)
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_shelx_res_checksum              46334
_shelx_hkl_checksum              12833