Structural studies of (prop-2-en-1-yl)bis[(pyridin-2-yl)methylidene]amine hetero-scorpionate copper complexes
Bussey, Katherine A.; Cavalier, Annie R.; Connell, Jennifer R.; Mraz, Margaret E.; Oshin, Kayode D.; Pintauer, Tomislav; Oliver, Allen G.; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615010335

data_2019975
_publ_section_title
;
 Structural studies of (prop-2-en-1-yl)bis[(pyridin-2-yl)methylidene]amine
 hetero-scorpionate copper complexes
;
_journal_coeditor_code           SK3587
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615010335
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cu Cl (C15 H17 N3)] Cl O4'
_chemical_formula_moiety         'C15 H17 Cl Cu N3 +, Cl O4 -'
_chemical_formula_sum            'C15 H17 Cl2 Cu N3 O4'
_chemical_formula_weight         437.76
_chemical_name_systematic
'Chlorido{(prop-2-en-1-yl)bis[pyridin-2-yl)methylidene]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}copper(II) perchlorate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.677(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4260(12)
_cell_length_b                   14.832(2)
_cell_length_c                   14.007(2)
_cell_measurement_reflns_used    4302
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0675
_cell_measurement_theta_min      2.736
_cell_volume                     1714.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_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 0.948
_diffrn_measurement_device_type  'Bruker SMART 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  0.0534
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10763
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.561
_diffrn_reflns_theta_min         2.747
_exptl_absorpt_coefficient_mu    1.612
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_correction_T_min  0.6200
_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    1.696
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.644
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1902 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                4766
_reflns_number_total             5553
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3587sup1.cif
_cod_data_source_block           4
_cod_database_code               2019975
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.907
_shelx_hkl_checksum              51583
_shelx_res_checksum              69537
_cod_database_fobs_code 2019975