Revisiting the structure and properties of mid-valent monopentamethylcyclopentadienylchromium complexes.
Calvo-Molina, Adrián; Jover, Jesús; Pérez-Redondo, Adrián; Yélamos, Carlos; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8190–8203; doi:10.1039/d5dt00620a

data_7718455
_publ_section_title
;
 Revisiting the structure and properties of mid-valent
 monopentamethylcyclopentadienylchromium complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8190
_journal_page_last               8203
_journal_paper_doi               10.1039/d5dt00620a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H76 Al4 Cr4, 1.5(C7 H8)'
_chemical_formula_sum            'C50.5 H88 Al4 Cr4'
_chemical_formula_weight         1011.12
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Pyrophoric
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2024-07-05T11:34:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2025-01-21 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.0970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1459(5)
_cell_length_b                   21.5739(8)
_cell_length_c                   18.3597(6)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.2
_cell_measurement_wavelength     0.71073
_cell_volume                     5457.3(3)
_computing_cell_refinement       'SAINT V8.40B integration software'
_computing_data_collection       'Apex3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type
;
Bruker AXS D8 Venture diffractometer with PhotonIII_C14 charge-integrating and 
photon counting pixel array detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_orient_matrix_UB_11      -0.004233
_diffrn_orient_matrix_UB_12      -0.043745
_diffrn_orient_matrix_UB_13      -0.018466
_diffrn_orient_matrix_UB_21      -0.072445
_diffrn_orient_matrix_UB_22      0.002827
_diffrn_orient_matrix_UB_23      -0.01254
_diffrn_orient_matrix_UB_31      0.001305
_diffrn_orient_matrix_UB_32      0.015063
_diffrn_orient_matrix_UB_33      -0.051274
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            152986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.9
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.87
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2156
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
The complex crystallized with one and half molecule of toluene, which
were found in the Fourier map, but it was not possible to get a sensible
chemical model for them, so Squeeze procedure was used to remove their
contribution to the structure factors.
;
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     517
_refine_ls_number_reflns         12518
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+3.0491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0
_reflns_number_gt                10934
_reflns_number_total             12518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00620a3.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7718451--7718458.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C50.50 H88 Al4 Cr4'
_cod_database_code               7718455
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20