Cyclopentadienyl and Alkynyl Copper(I) Derivatives with the [{Ti(η5-C5Me5)(μ-NH)}3(μ3-N)] Metalloligand
Martínez-Espada, Noelia; Mena, Miguel; Mosquera, Marta E. G.; Pérez-Redondo, Adrián; Yélamos, Carlos; Organometallics 29 (2010) 6732–; doi:10.1021/om100824q

data_4067093
_publ_section_title
;
 Cyclopentadienyl and Alkynyl Copper(I) Derivatives with the
 [{Ti(\h5-C5Me5)(\m-NH)}3(\m3-N)] Metalloligand
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6732
_journal_paper_doi               10.1021/om100824q
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C90 H120 Cu4 N8 Ti6'
_chemical_formula_sum            'C90 H120 Cu4 N8 Ti6'
_chemical_formula_weight         1855.5
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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             2010-07-22T18:07:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.95(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3197(15)
_cell_length_b                   17.216(7)
_cell_length_c                   23.233(15)
_cell_measurement_reflns_used    116
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.857
_cell_measurement_theta_min      3.4
_cell_measurement_wavelength     0.71073
_cell_volume                     4525(4)
_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)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.124
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            87958
_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         3.08
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.527(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         20367
_refine_ls_number_restraints     767
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                14044
_reflns_number_total             20367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100824q_si_002.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4067093