Copper and Silver Complexes Containing Organic Azide Ligands: Syntheses, Structures, and Theoretical Investigation of [HB(3,5-(CF3)2Pz)3]CuNNN(1-Ad) and [HB(3,5-(CF3)2Pz)3]AgN(1-Ad)NN (Where Pz = Pyrazolyl and 1-Ad = 1-Adamantyl)
H. V. Rasika Dias; Sharon A. Polach; Sor-Koon Goh; Edet F. Archibong; Dennis S. Marynick; Inorganic Chemistry 39 (2000) 3894–3901; doi:10.1021/ic0004232

data_4321267
_publ_section_title
;
 Copper and Silver Complexes Containing Organic Azide Ligands: Syntheses,
 Structures, and Theoretical Investigation of
 [HB(3,5-(CF3)2Pz)3]CuNNN(1-Ad) and [HB(3,5-(CF3)2Pz)3]AgN(1-Ad)NN (Where
 Pz = Pyrazolyl and 1-Ad = 1-Adamantyl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3894
_journal_page_last               3901
_journal_paper_doi               10.1021/ic0004232
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C28.5 H23 B Cu F18 N9'
_chemical_formula_weight         907.91
_chemical_name_common            '[HB(3,5-(CF3)2Pz)3]CuN3Ad/0.5(C7H8)'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.621(10)
_cell_angle_beta                 108.817(11)
_cell_angle_gamma                90.081(9)
_cell_formula_units_Z            2
_cell_length_a                   10.4911(12)
_cell_length_b                   11.4778(12)
_cell_length_c                   16.139(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      5.35
_cell_volume                     1810.4(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5364
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.80
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.7360
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         4436
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.9396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                3773
_reflns_number_total             4436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0004232_1.cif
_cod_data_source_block           rd222
_cod_original_cell_volume        1810.5(4)
_cod_original_formula_sum        'C28.50 H23 B Cu F18 N9'
_cod_database_code               4321267