Copper(I) Complexes with a NS2-Macrocyclic Ligand Bearing a Pendant Naphthyl Group: Structures of {N-[2-(1-Naphthyl)ethyl]-1-aza-4,8-dithiacyclodecane}copper(I)-Ligand, where Ligand = η2-Naphthalene, Acetonitrile, or Triphenylphosphine
Rebecca R. Conry; William S. Striejewske; A. Alex Tipton; Inorganic Chemistry 38 (1999) 2833–2843; doi:10.1021/ic981418p

data_4322081
_publ_contact_author_address
;   University of Nevada, Reno
    Department of Chemistry 216
    Reno, Nevada  89557   USA
;
_publ_contact_author_email       conry@chem.unr.edu
_publ_contact_author_name        'Rebecca R. Conry'
_publ_section_title
;
 Copper(I) Complexes with a NS2-Macrocyclic Ligand Bearing a Pendant
 Naphthyl Group: Structures of
 {N-[2-(1-Naphthyl)ethyl]-1-aza-4,8-dithiacyclodecane}copper(I)-Ligand,
 where Ligand = \h2-Naphthalene, Acetonitrile, or Triphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2833
_journal_page_last               2843
_journal_paper_doi               10.1021/ic981418p
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C22 H31 Cu F6 N P S2'
_chemical_formula_weight         582.11
_chemical_name_common            'Complex 2'
_chemical_name_systematic
;  [(N-(2-(1-naphthyl)ethyl)-1-aza-4,8-dithiacyclodecane)copper(I)]
 hexafluorophosphate 
;
_chemical_temperature_decomposition 470
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL generated with manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.431(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7318(15)
_cell_length_b                   8.9164(10)
_cell_length_c                   17.205(2)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      12.92
_cell_measurement_theta_min      1.89
_cell_volume                     2356.8(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measurement_device       '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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5287
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        'not significant'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.85
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_obs          0.0587
_refine_ls_shift/esd_max         -0.016
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+2.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1545
_refine_ls_wR_factor_obs         0.1285
_reflns_number_observed          2517
_reflns_number_total             4153
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981418p_2.cif
_cod_data_source_block           complex2.IC981418P
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+2.4439P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+2.4439P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322081