Crystal structures, electron spin resonance, and thermogravimetric analysis of three mixed-valence copper cyanide polymers.
Corfield, Peter W. R.; Elsayed, Ahmed; DaCunha, Tristan; Bender, Christopher; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624003371

data_2312480
_publ_section_title
;
 Crystal structures, electron spin resonance, and thermogravimetric
 analysis of three mixed-valence copper cyanide polymers.
;
_journal_coeditor_code           DG3052
_journal_issue                   6
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624003371
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Cu3 (C N)4 (C2 H7 N1 O1)2]'
_chemical_formula_moiety         'C8 H14 Cu3 N6 O2'
_chemical_formula_sum            'C8 H14 Cu3 N6 O2'
_chemical_formula_weight         416.88
_chemical_name_systematic
;
Poly[bis(2-aminoethanol)tetra-\m-cyanido-tricopper(II)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 117.3580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5158(2)
_cell_length_b                   8.8022(2)
_cell_length_c                   9.3589(2)
_cell_measurement_reflns_used    2164
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      1.0
_cell_volume                     696.22(3)
_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) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.046
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27010
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         28.810
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Otwinowski & Minor,1997)
;
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.533
_refine_ls_extinction_coef       0.0030(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                1049
_reflns_number_total             1740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3052.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312480
_shelx_estimated_absorpt_t_min   0.284
_shelx_estimated_absorpt_t_max   0.435
_shelx_hkl_checksum              91832
_shelx_res_checksum              44470