A new class of macrocyclic complexes formed via nickel-promoted macrocyclisation of dioxime with dinitrile
Pavlishchuk, Vitaly V.; Kolotilov, Sergey V.; Addison, Anthony W.; Prushan, Michael J.; Butcher, Raymond J.; Thompson, Laurence K.; Chemical Communications  (2002) 468–; doi:10.1039/b111191b

data_7114331
_publ_section_title
;
 A new class of macrocyclic complexes formed via nickel-promoted
 macrocyclisation of dioxime with dinitrile
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              468
_journal_paper_doi               10.1039/b111191b
_journal_year                    2002
_chemical_formula_sum            'C32 H46 Cl4 N8 Ni2 O23 S4'
_chemical_formula_weight         1298.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.0310(10)
_cell_angle_beta                 100.5090(10)
_cell_angle_gamma                104.5620(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9847(2)
_cell_length_b                   12.1783(2)
_cell_length_c                   19.8496(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2693.67(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.782
_diffrn_measured_fraction_theta_max 0.782
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12315
_diffrn_reflns_theta_full        66.81
_diffrn_reflns_theta_max         66.81
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    4.874
_exptl_absorpt_correction_T_max  0.6457
_exptl_absorpt_correction_T_min  0.3363
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         7493
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.416
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1681P)^2^+0.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2358
_reflns_number_gt                5515
_reflns_number_total             7493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111191b.txt
_cod_data_source_block           sk41199c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2693.66(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114331