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_2019972
_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)], 0.18H2 O'
_chemical_formula_moiety         'C15 H17 Cl Cu N3, 0.18(H2 O)'
_chemical_formula_sum            'C15 H17.355 Cl Cu N3 O0.18'
_chemical_formula_weight         341.52
_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(I) 0.18-hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_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            8
_cell_length_a                   29.2238(13)
_cell_length_b                   8.2252(4)
_cell_length_c                   12.8789(6)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.47
_cell_volume                     3095.7(2)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_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 0.961
_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  0.0304
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37660
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.638
_diffrn_reflns_theta_min         2.108
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.8371
_exptl_absorpt_correction_T_min  0.6291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.428
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.504(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10665
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.6853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                8406
_reflns_number_total             10665
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3587sup1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C15 H17.355 Cl1 Cu1 N3 O0.18'
_cod_database_code               2019972
_cod_database_fobs_code          2019972
_shelx_estimated_absorpt_t_min   0.629
_shelx_estimated_absorpt_t_max   0.837
_shelx_hkl_checksum              30454
_shelx_res_checksum              41147