Copper(I) and Silver(I) Complexes Supported by the Tridentate [{Ti(η5-C5Me5)(μ-NH)}3(μ3-N)] Metalloligand
Avelino Martín; Noelia Martínez-Espada; Miguel Mena; Adrián Pérez-Redondo; Carlos Yélamos; Inorganic Chemistry 52 (2013) 918–930; doi:10.1021/ic302113k

data_4333597
_publ_section_title
;
 Copper(I) and Silver(I) Complexes Supported by the Tridentate
 [{Ti(\h5-C5Me5)(\m-NH)}3(\m3-N)] Metalloligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              918
_journal_page_last               930
_journal_paper_doi               10.1021/ic302113k
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C86 H120 Cu2 N8 P2 Ti6, C2 H4 Cl4, 2(C F3 O3 S)'
_chemical_formula_sum            'C90 H124 Cl4 Cu2 F6 N8 O6 P2 S2 Ti6'
_chemical_formula_weight         2210.31
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2012-04-09T14:11:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                89.017(14)
_cell_angle_beta                 71.718(13)
_cell_angle_gamma                68.809(13)
_cell_formula_units_Z            1
_cell_length_a                   12.530(3)
_cell_length_b                   12.621(3)
_cell_length_c                   18.7029(18)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     2603.0(10)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57759
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_description       prism
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11946
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+1.3336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                7170
_reflns_number_total             11946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302113k_si_001_6.cif
_cod_data_source_block           18
_cod_original_cell_volume        2602.9(8)
_cod_database_code               4333597