Poly[tris(2-aminobutan-1-ol)copper(II) [hexakis-μ2-cyanido-κ12 C:N-tetracopper(I)] bis(2-aminobutan-1-olato)aquacopper(II) monohydrate]
Corfield, Peter W. R.; Salvi, Paul; IUCrData 9 (2024) x240845–; doi:10.1107/S2414314624008459

data_1572441
_publ_section_title
;
 Poly[tris(2-aminobutan-1-ol)copper(II) [hexakis-\m2-cyanido-\k12
 C:N-tetracopper(I)] bis(2-aminobutan-1-olato)aquacopper(II) monohydrate]
;
_journal_coeditor_code           BH4088
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x240845
_journal_paper_doi               10.1107/S2414314624008459
_journal_volume                  9
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_iupac
;
[Cu (C4 H11 N1 O1)3] [Cu4 (C N)6], [Cu (C4 H10 N1 O1)2 (H2 O1)], H2 O
;
_chemical_formula_moiety
;
C8 H22 Cu N2 O3 2+, C6 Cu4 N6 2-, C12 H33 Cu N3 O3, H2 O
;
_chemical_formula_sum            'C26 H57 Cu6 N11 O7'
_chemical_formula_weight         1017.06
_chemical_name_systematic
;
Poly[tris(2-aminobutan-1-ol)copper(II)
[hexakis-\m~2~-cyanido-\k^12^<i>C</i>:<i>N</i>-tetracopper(I)]
bis(2-aminobutan-1-olato)aquacopper(II) monohydrate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 91.4860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1008(2)
_cell_length_b                   14.9561(3)
_cell_length_c                   12.7221(2)
_cell_measurement_reflns_used    5040
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2111.47(7)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41170
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.356
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2729 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8587
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0396P)^2^+0.5870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                6363
_reflns_number_total             8587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bh4088.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1572441
_shelx_estimated_absorpt_t_min   0.436
_shelx_estimated_absorpt_t_max   0.889
_shelx_hkl_checksum              43319
_shelx_res_checksum              49644