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_7045836
_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            'C41.91 H39.81 Cl3.81 Fe2 Hf2 Se4'
_chemical_formula_weight         1462.90
_chemical_name_systematic
Bis(1,1'-ferrocenyldiselenolato)bis{bis(cyclopentadienyl)hafnium}
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     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                90
_cell_angle_beta                 94.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.648(2)
_cell_length_b                   23.329(5)
_cell_length_c                   15.788(3)
_cell_measurement_reflns_used    8227
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      73.4250
_cell_measurement_theta_min      3.3650
_cell_volume                     4277.7(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      155(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71499
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.730
_diffrn_reflns_theta_min         3.387
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    20.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.893
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+17.4514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8227
_reflns_number_total             8598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00300a2.cif
_cod_data_source_block           cmpd3
_cod_depositor_comments
'Adding full bibliography for 7045833--7045836.cif.'
_cod_original_cell_volume        4277.5(14)
_cod_database_code               7045836
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.429
_shelx_res_checksum              45626