Aryl-Linked Salicylaldoxime-Based Copper(II) Helicates and "Boxes": Synthesis, X-ray Analysis, and Anion Influence on Complex Structure
Ajay Pal Singh Pannu; James R. Stevens; Paul G. Plieger; Inorganic Chemistry 52 (2013) 9327–9337; doi:10.1021/ic400829d

data_4335729
_publ_contact_author_address
;
Institute of Fundamental Sciences
Massey University
Private Bag 11 222
Palmerston North
4442
NEW ZEALAND
;
_publ_contact_author_email       p.g.plieger@massey.ac.nz
_publ_contact_author_name        P.Plieger
_publ_section_title
;
 Aryl-Linked Salicylaldoxime-Based Copper(II) Helicates and "Boxes":
 Synthesis, X-ray Analysis, and Anion Influence on Complex Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9327
_journal_page_last               9337
_journal_paper_doi               10.1021/ic400829d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C34 H44 Cu N4 O4, C6 H14 O'
_chemical_formula_sum            'C40 H58 Cu N4 O5'
_chemical_formula_weight         738.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.740(6)
_cell_angle_beta                 69.547(5)
_cell_angle_gamma                68.645(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5153(14)
_cell_length_b                   13.7564(17)
_cell_length_c                   14.434(2)
_cell_measurement_reflns_used    16716
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      6.5
_cell_volume                     1989.2(5)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 2.0 rc14 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 2.0 rc14 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 2.0 rc14 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type
; 
Rigaku CrystalClear-SM Expert 2.0 rc14 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.1336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24934
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         6.51
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.619
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0732P)^2^+0.2618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                4510
_reflns_number_total             6519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400829d_si_002_5.cif
_cod_data_source_block           CCDC926414
_cod_original_cell_volume        1989.2(4)
_cod_database_code               4335729