Synthesis of 14-oxa-1,4,8,11-tetraazabicyclo[9.5.3]nonadecane (L1) and a Spectroscopic and Structural Study of [Ni(L1)(ClO4)](ClO4) and of the Macrobicyclic Precursor Diamide Complex, [Ni(HL2)](ClO4); Chloride Substitution Kinetics of the Corresponding [Ni(III)(L1)]3+ Species
M. Rodopoulos; T. Rodopoulos; J. N. Bridson; L. I. Elding; S. J. Rettig; A. McAuley; Inorganic Chemistry 40 (2001) 2737–2742; doi:10.1021/ic001163r

data_4319742
_publ_contact_author_address
;
Chemistry Department, University of
Victoria, Victoria, BC
;
_publ_contact_author_email       amcauley@uvic.ca
_publ_contact_author_fax         '250 721-7147'
_publ_contact_author_name        A.McAuley
_publ_contact_author_phone       '250 721-7164'
_publ_section_title
;
 Synthesis of 14-oxa-1,4,8,11-tetraazabicyclo[9.5.3]nonadecane (L1) and a
 Spectroscopic and Structural Study of [Ni(L1)(ClO4)](ClO4) and of the
 Macrobicyclic Precursor Diamide Complex, [Ni(HL2)](ClO4); Chloride
 Substitution Kinetics of the Corresponding [Ni(III)(L1)]3+ Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2737
_journal_page_last               2742
_journal_paper_doi               10.1021/ic001163r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C14 H24 Cl N4 Ni O7'
_chemical_formula_weight         454.52
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             1998-09-18
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1590(3)
_cell_length_b                   13.235(2)
_cell_length_c                   18.0195(6)
_cell_measurement_reflns_used    14324
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.0
_cell_volume                     3615.2(6)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution    'DIRDIF92 PATTY (Beurskens, 1992)'
_diffrn_ambient_temperature      180.2
_diffrn_detector_area_resol_mean 11.76
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.09213
_diffrn_reflns_av_sigmaI/netI    0.180
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33886
_diffrn_reflns_reduction_process 'Lp corrections applied'
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_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
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_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
d*TREK (MSC, 1996-1998)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
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_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.33
_refine_diff_density_min         -1.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.136
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/su_max          0.0190
_refine_ls_shift/su_mean         0.0310
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0826
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                1703
_reflns_number_total             5137
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic001163r.cif
_cod_data_source_block           C14H24ClN4O7Ni
_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_original_cell_volume        3615.3(7)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C14 H24 Cl N4 O7 Ni '
_cod_database_code               4319742