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_4335726
_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
'3(C68 H92 Br2 Cu2 N8 O8), 6(B F4), 2(C3 H6 O)'
_chemical_formula_sum            'C210 H288 B6 Br6 Cu6 F24 N24 O26'
_chemical_formula_weight         4946.20
_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
_cell_angle_alpha                99.607(7)
_cell_angle_beta                 96.215(7)
_cell_angle_gamma                106.635(7)
_cell_formula_units_Z            1
_cell_length_a                   14.5994(12)
_cell_length_b                   19.6925(17)
_cell_length_c                   27.748(2)
_cell_measurement_reflns_used    7875
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      61.7
_cell_measurement_theta_min      6.5
_cell_volume                     7432.9(11)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      161(2)
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_av_sigmaI/netI    0.2394
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73025
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         6.47
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2554
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Diffuse solvent corresponding to 14 acetone molecules / cell (448e)
was squeezed out
;
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         20103
_refine_ls_number_restraints     1070
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.2414
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2732
_refine_ls_wR_factor_ref         0.3336
_reflns_number_gt                6244
_reflns_number_total             20103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400829d_si_002_2.cif
_cod_data_source_block           CCDC926416
_cod_original_cell_volume        7433.0(11)
_cod_database_code               4335726