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_2311351
_publ_section_title
;
 Crystal structures of two mixed-valence copper cyanide complexes with
 <i>N</i>-methyl-ethylenedi-amine.
;
_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          '[Cu2 (C N)3 (C3 H10 N2)2], H2 O'
_chemical_formula_moiety         'C9 H20 Cu2 N7, H2 O'
_chemical_formula_sum            'C9 H22 Cu2 N7 O'
_chemical_formula_weight         371.42
_chemical_name_common
;
bis(N-methylethylenediamine)copper(II)-\m-cyano-copper(I)dicyanide
;
_chemical_name_systematic
'[(<i>N</i>-Methylethylenediamine-\k^2^<i>N</i>,<i>N</i>')copper(II)]-\m~2~-cyanido-\k^2^<i>C</i>:<i>N</i>-[bis(cyanido-\k<i>C</i>)copper(I)] monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014/7 '
_cell_angle_alpha                94.6851(14)
_cell_angle_beta                 101.8607(12)
_cell_angle_gamma                108.3780(13)
_cell_formula_units_Z            2
_cell_length_a                   7.5621(2)
_cell_length_b                   8.8689(2)
_cell_length_c                   12.8098(3)
_cell_measurement_reflns_used    3501
_cell_measurement_temperature    300.0(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.83
_cell_volume                     787.91(3)
_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
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      300.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.029
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24810
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.987
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_T_max  0.39
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(SCALEPACK; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      1.570(5)
_exptl_crystal_density_method
; flotation in 1,2-dibromopropane/1,2,3-trichloropropane mixtures.
Four independent determinations were made.
;
_exptl_crystal_description
;
block cut from large elongated plate
;
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.259
_refine_ls_extinction_coef       0.0187(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                3387
_reflns_number_total             3611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2594sup1.cif
_cod_data_source_block           II
_cod_database_code               2311351
_shelx_hkl_checksum              52070
_shelx_res_checksum              24785