Crystal structure of {(but-3-en-1-yl)bis[(pyridin-2-yl)methyl]amine-κ^3^<i>N</i>,<i>N</i>',<i>N</i>''}dichloridocopper(II) diethyl ether hemisolvate
Bussey, Katherine A.; Connell, Jennifer R.; McGlone, Annie R.; Mraz, Margaret E.; Oshin, Kayode D.; Pintauer, Tomislav; Oliver, Allen G.; Acta Crystallographica Section E 71 (2015) 309–311; doi:10.1107/S2056989015003448

data_2240456
_publ_section_title
;
 Crystal structure of
 {(but-3-en-1-yl)bis[(pyridin-2-yl)methyl]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}dichloridocopper(II)
 diethyl ether hemisolvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              309
_journal_page_last               311
_journal_paper_doi               10.1107/S2056989015003448
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cu Cl2 (C16 H19 N3)], 0.5C4 H10 O'
_chemical_formula_moiety         'C16 H19 Cl2 Cu N3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C18 H24 Cl2 Cu N3 O0.5'
_chemical_formula_weight         424.84
_chemical_name_systematic
;{(But-3-en-1-yl)bis[(pyridin-2-yl)methyl]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''} dichloridocopper(II)
diethyl ether hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.7710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1614(13)
_cell_length_b                   11.5738(5)
_cell_length_c                   16.4530(7)
_cell_measurement_reflns_used    8841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.22
_cell_measurement_theta_min      2.22
_cell_volume                     3995.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and POV-Ray (Cason, 2013)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.606
_diffrn_reflns_theta_min         1.941
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.8396
_exptl_absorpt_correction_T_min  0.4705
_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    1.412
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0348P)^2^+2.0749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                5660
_reflns_number_total             6872
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2546sup1.cf
_cod_data_source_block           I
_cod_original_formula_sum        'C18 H24 Cl2 Cu1 N3 O0.5'
_cod_database_code               2240456
_cod_database_fobs_code          2240456
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.873
_shelx_hkl_checksum              67717
_shelx_res_checksum              12824