Solution-State and Solid-State Structural Characterization of Complexes of a New Macrocyclic Ligand Containing the 1,5-Diazacyclooctane Subunit
Chuanjiang Hu; Thoi D. Nguyen; Paul S. Wagenknecht; Lawrence C. Nathan; Inorganic Chemistry 42 (2003) 742–749; doi:10.1021/ic020495o

data_4313018
_publ_contact_author_address
;
         Department of Chemistry
         San Jose State University
         San Jose, CA 95192
;
_publ_contact_author_email       pwagen@jupiter.sjsu.edu
_publ_contact_author_fax         408-924-4945
_publ_contact_author_name        'Paul S. Wagenknecht'
_publ_contact_author_phone       408-924-5008
_publ_section_title
;
 Solution-State and Solid-State Structural Characterization of Complexes
 of a New Macrocyclic Ligand Containing the 1,5-Diazacyclooctane Subunit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              742
_journal_page_last               749
_journal_paper_doi               10.1021/ic020495o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C13 H28 N4 Ni, 2(C F3 O3 S)'
_chemical_formula_sum            'C15 H28 F6 N4 Ni O6 S2'
_chemical_formula_weight         597.24
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.060(2)
_cell_length_b                   13.818(2)
_cell_length_c                   15.638(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.052
_cell_measurement_theta_min      9.655
_cell_volume                     2369.6(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5303
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0.0%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Siemens SHELXTL'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4161
_refine_ls_number_restraints     314
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+3.8661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                3125
_reflns_number_total             4165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020495o_1.cif
_cod_data_source_block           nic3cy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2369.5(8)
_cod_database_code               4313018