[(1<i>RS</i>,7<i>RS</i>,8<i>RS</i>,14<i>RS</i>)-5,12-Dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene-κ^4^<i>N</i>^1,4,8,11^]nickel(II) perchlorate
Neil F. Curtis; David C. Weatherburn; Acta Crystallographica Section E 58 (2002) m423–m425; doi:10.1107/S1600536802012205

data_2201633
_publ_section_title
;[(1<i>RS</i>,7<i>RS</i>,8<i>RS</i>,14<i>RS</i>)-5,12-Dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene-\k^4^<i>N</i>^1,4,8,11^]nickel(II)
 perchlorate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m423
_journal_page_last               m425
_journal_paper_doi               10.1107/S1600536802012205
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni (C24 H32 N4)] (ClO4)'
_chemical_formula_moiety         'C24 H32 N4 Ni 1+, 2Cl O4 1-'
_chemical_formula_sum            'C24 H32 Cl2 N4 Ni O8'
_chemical_formula_weight         634.13
_chemical_name_systematic
;
(1RS,7RS,8RS,14SR-5,12-Dimethyl-7,14-diphenyl-1,4,8,11-
tetraazacyclotetradeca-4,11-diene-N^1^,N^4^,N^8^,N^11^)nickel(II)
Perchlorate
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.66(2)
_cell_length_b                   29.400(10)
_cell_length_c                   9.267(4)
_cell_measurement_reflns_used    4795
_cell_measurement_temperature    158.2(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.4
_cell_volume                     11078(8)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-32 (Johnson, 1999)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_av_sigmaI/netI    0.167
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            34536
_diffrn_reflns_theta_full        26.3
_diffrn_reflns_theta_max         26.3
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.36
_refine_ls_abs_structure_details 'Flack (1983), 1661 Friedel pairs [CHECK]'
_refine_ls_abs_structure_Flack   0.020(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.76
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4658
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.76
_refine_ls_R_factor_all          0.092
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.04P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.083
_reflns_number_gt                2435
_reflns_number_total             4658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6068.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2201633