Macrocycles containing 1,1'-ferrocenyldiselenolato ligands on group 4 metallocenes.
Sanchez-Perez, Clara; Knapp, Caroline E.; Karjalainen, Minna M.; Oilunkaniemi, Raija; Carmalt, Claire J.; Laitinen, Risto S.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5415–5421; doi:10.1039/c8dt00300a

data_7045833
_publ_section_title
;
 Macrocycles containing 1,1'-ferrocenyldiselenolato ligands on group 4
 metallocenes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5415
_journal_page_last               5421
_journal_paper_doi               10.1039/c8dt00300a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C57 H52.5 Fe2 Se4 Ti2'
_chemical_formula_weight         1260.83
_chemical_name_systematic
Bis(1,1'-ferrocenyldiselenolato)bis{bis(cyclopentadienyl)titanium}
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                96.90(3)
_cell_angle_beta                 101.22(3)
_cell_angle_gamma                90.15(3)
_cell_formula_units_Z            2
_cell_length_a                   11.413(2)
_cell_length_b                   14.514(3)
_cell_length_c                   15.645(3)
_cell_measurement_reflns_used    8290
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      2.925
_cell_volume                     2522.7(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2008)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Nonius Kappaccd'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34338
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.792
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Sheldrick 2008)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             1253
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/toluene'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0064(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9831
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+5.7538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8290
_reflns_number_total             9831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00300a2.cif
_cod_data_source_block           cmpd1
_cod_depositor_comments
'Adding full bibliography for 7045833--7045836.cif.'
_cod_original_formula_sum        'C57 H52.50 Fe2 Se4 Ti2'
_cod_database_code               7045833
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.582
_shelx_estimated_absorpt_t_max   0.659
_shelx_res_checksum              42054