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_4335728
_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_absolute_configuration unk
_chemical_formula_moiety         'C68 H92 Cu2 N9 O11, 3(N O3)'
_chemical_formula_sum            'C68 H92 Cu2 N12 O20'
_chemical_formula_weight         1524.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.297(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4408(19)
_cell_length_b                   20.2715(4)
_cell_length_c                   19.0446(13)
_cell_measurement_reflns_used    16990
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.7
_cell_measurement_theta_min      6.5
_cell_volume                     4239.4(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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           Copper
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49913
_diffrn_reflns_theta_full        72.04
_diffrn_reflns_theta_max         72.036
_diffrn_reflns_theta_min         6.52
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The structure contained multiple diffuse methanol molecules. 
149 electrons per cell were squeezed out corresponding to
eight methanol molecules per cell (144e)
;
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.0015(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   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         14261
_refine_ls_number_restraints     721
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                9962
_reflns_number_total             14261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400829d_si_002_4.cif
_cod_data_source_block           CCDC926417
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoclinc' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4335728