Crystal structures of two mixed-valence copper cyanide complexes with <i>N</i>-methyl-ethylenedi-amine.
Corfield, Peter W. R.; Sabatino, Alexander; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 141–146; doi:10.1107/S2056989017000111

data_2311350
_publ_section_title
;
 Crystal structures of two mixed-valence copper cyanide complexes with
 <i>N</i>-methyl-ethylenedi-amine.
;
_journal_coeditor_code           PK2594
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              141
_journal_page_last               146
_journal_paper_doi               10.1107/S2056989017000111
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cu4 (C N)5 (C3 H10 N2)2]'
_chemical_formula_moiety         'C11 H20 Cu4 N9'
_chemical_formula_sum            'C11 H20 Cu4 N9'
_chemical_formula_weight         532.52
_chemical_name_systematic
;Poly[bis(\m~3~-cyanido-\k^3^<i>C</i>:<i>C</i>:<i>N</i>)tris(\m~2~-cyanido-\k^2^<i>C</i>:<i>N</i>)bis(<i>N</i>-methylethane-1,2-diamine\-
\k^2^<i>N</i>,<i>N</i>')tricopper(I)copper(II)]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.509(2)
_cell_length_b                   8.2306(13)
_cell_length_c                   11.100(2)
_cell_measurement_reflns_used    474
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      20.18
_cell_measurement_theta_min      1.83
_cell_volume                     1782.3(5)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>KappaCCD Server Software</i> (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>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      303.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Enraf--Nonius KappaCCD'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15054
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_min         2.088
_exptl_absorpt_coefficient_mu    4.721
_exptl_absorpt_correction_T_max  0.146
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(SCALEPACK; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_meas      2.01(7)
_exptl_crystal_density_method
; flotation in 1,2-dibromopropane/1,2,3-trichloropropane mixtures.
Three independent determinations were made.
;
_exptl_crystal_description
;
block cut from large polyhedral crystal
;
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.383
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1806 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.010(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                3964
_reflns_number_total             4062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2594sup1.cif
_cod_data_source_block           I
_cod_database_code               2311350
_shelx_hkl_checksum              18526
_shelx_res_checksum              12437