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_4335727
_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         'C68 H92 Br2 Cu2 N8 O8, 2(C H3 O), 2(Br)'
_chemical_formula_sum            'C70 H98 Br4 Cu2 N8 O10'
_chemical_formula_weight         1658.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.245(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.7715(16)
_cell_length_b                   19.5276(4)
_cell_length_c                   19.8252(4)
_cell_measurement_reflns_used    32576
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.5
_cell_volume                     8801.6(7)
_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      140(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            90481
_diffrn_reflns_theta_full        72.09
_diffrn_reflns_theta_max         72.09
_diffrn_reflns_theta_min         6.50
_exptl_absorpt_coefficient_mu    3.132
_exptl_absorpt_correction_T_max  0.4339
_exptl_absorpt_correction_T_min  0.2638
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       Block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
The unit cell contained a large number of partially occupied
diffuse methanol solvent molecules. Total electron count = 272e/cell
corresponding to 15 MeOH solvent molecules per cell (270e).
;
_refine_diff_density_max         1.056
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         16757
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                11558
_reflns_number_total             16757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400829d_si_002_3.cif
_cod_data_source_block           CCDC926415
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4335727