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#$Date: 2025-07-06 19:20:30 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300863 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/84/7718457.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7718457
loop_
_publ_author_name
'Calvo-Molina, Adrián'
'Jover, Jesús'
'Pérez-Redondo, Adrián'
'Yélamos, Carlos'
_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         'C32 H42 Cl2 Cr2 N2, 2(C6 H5 F)'
_chemical_formula_sum            'C44 H52 Cl2 Cr2 F2 N2'
_chemical_formula_weight         821.77
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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             2024-07-04T17:42:28-00:00
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8952(10)
_cell_length_b                   17.2829(14)
_cell_length_c                   19.3699(16)
_cell_measurement_reflns_used    7259
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     3982.1(6)
_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       'κ-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      0.00176
_diffrn_orient_matrix_UB_12      0.04417
_diffrn_orient_matrix_UB_13      -0.033331
_diffrn_orient_matrix_UB_21      -0.076908
_diffrn_orient_matrix_UB_22      -0.014226
_diffrn_orient_matrix_UB_23      -0.016539
_diffrn_orient_matrix_UB_31      -0.033904
_diffrn_orient_matrix_UB_32      0.034562
_diffrn_orient_matrix_UB_33      0.035788
_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  0.1446
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112624
_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         26.426
_diffrn_reflns_theta_min         2.712
_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    0.723
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: fluorobenzene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.164
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0544
_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/[σ²(Fo²)+(0.0842P)²+9.5844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0
_reflns_number_gt                2988
_reflns_number_total             4088
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00620a3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7718451--7718458.cif.'
_cod_database_code               7718457
_shelx_shelxl_version_number     2018/3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
H1 H 0.446(5) 0.545(3) 0.584(3) 0.065(17) Uiso 1 1 d . . . . .
C1 C 0.2969(3) 0.5058(2) 0.56994(19) 0.0262(8) Uani 1 1 d . . . . .
C2 C 0.2571(3) 0.5549(2) 0.6220(2) 0.0336(9) Uani 1 1 d . . . . .
H2 H 0.30687 0.590459 0.643635 0.04 Uiso 1 1 calc R U . . .
C3 C 0.1451(4) 0.5519(3) 0.6422(2) 0.0423(11) Uani 1 1 d . . . . .
H3 H 0.118604 0.585416 0.677489 0.051 Uiso 1 1 calc R U . . .
C4 C 0.0721(4) 0.5005(3) 0.6113(2) 0.0437(11) Uani 1 1 d . . . . .
H4 H -0.004609 0.498686 0.624895 0.052 Uiso 1 1 calc R U . . .
C5 C 0.1112(4) 0.4520(3) 0.5607(3) 0.0429(10) Uani 1 1 d . . . . .
H5 H 0.061037 0.416575 0.539226 0.051 Uiso 1 1 calc R U . . .
C6 C 0.2229(3) 0.4538(2) 0.5403(2) 0.0344(9) Uani 1 1 d . . . . .
H6 H 0.24881 0.419127 0.505733 0.041 Uiso 1 1 calc R U . . .
C11 C 0.6433(3) 0.4232(2) 0.61933(19) 0.0273(8) Uani 1 1 d . . . . .
C12 C 0.5358(3) 0.3981(2) 0.64301(18) 0.0268(8) Uani 1 1 d . . . . .
C13 C 0.5085(3) 0.3286(2) 0.6082(2) 0.0279(8) Uani 1 1 d . . . . .
C14 C 0.6009(3) 0.3093(2) 0.5646(2) 0.0284(8) Uani 1 1 d . . . . .
C15 C 0.6834(3) 0.3672(2) 0.5717(2) 0.0292(8) Uani 1 1 d . . . . .
C16 C 0.7084(4) 0.4902(2) 0.6473(2) 0.0376(10) Uani 1 1 d . . . . .
H16A H 0.747126 0.47451 0.689709 0.056 Uiso 1 1 calc R U . . .
H16B H 0.656905 0.532961 0.657518 0.056 Uiso 1 1 calc R U . . .
H16C H 0.763839 0.507035 0.613038 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4660(4) 0.4365(2) 0.6980(2) 0.0351(9) Uani 1 1 d . . . . .
H17A H 0.386156 0.426635 0.689088 0.053 Uiso 1 1 calc R U . . .
H17B H 0.479942 0.492362 0.697434 0.053 Uiso 1 1 calc R U . . .
H17C H 0.486394 0.415462 0.743285 0.053 Uiso 1 1 calc R U . . .
C18 C 0.4035(3) 0.2822(2) 0.6176(2) 0.0370(9) Uani 1 1 d . . . . .
H18A H 0.405494 0.256262 0.662634 0.056 Uiso 1 1 calc R U . . .
H18B H 0.398072 0.243303 0.580955 0.056 Uiso 1 1 calc R U . . .
H18C H 0.338004 0.316526 0.61555 0.056 Uiso 1 1 calc R U . . .
C19 C 0.6108(4) 0.2371(2) 0.5218(2) 0.0406(10) Uani 1 1 d . . . . .
H19A H 0.663461 0.246148 0.483697 0.061 Uiso 1 1 calc R U . . .
H19B H 0.536896 0.223458 0.503062 0.061 Uiso 1 1 calc R U . . .
H19C H 0.638605 0.194664 0.55065 0.061 Uiso 1 1 calc R U . . .
C20 C 0.7991(3) 0.3650(3) 0.5406(2) 0.0399(10) Uani 1 1 d . . . . .
H20A H 0.845755 0.328053 0.566181 0.06 Uiso 1 1 calc R U . . .
H20B H 0.83301 0.416546 0.543152 0.06 Uiso 1 1 calc R U . . .
H20C H 0.793901 0.348785 0.492223 0.06 Uiso 1 1 calc R U . . .
Cl1 Cl 0.42173(8) 0.35374(5) 0.44551(5) 0.0294(2) Uani 1 1 d . . . . .
Cr1 Cr 0.52328(5) 0.42208(3) 0.52949(3) 0.02119(19) Uani 1 1 d . . . . .
N1 N 0.4119(3) 0.51107(18) 0.55020(16) 0.0259(7) Uani 1 1 d . . . . .
C100 C 0.7256(4) 0.2754(3) 0.7299(2) 0.0481(12) Uani 1 1 d . . . . .
C101 C 0.6569(4) 0.3035(3) 0.7814(2) 0.0522(13) Uani 1 1 d . . . . .
H101 H 0.66916 0.352918 0.801602 0.063 Uiso 1 1 calc R U . . .
C102 C 0.5695(4) 0.2564(4) 0.8023(2) 0.0597(16) Uani 1 1 d . . . . .
H102 H 0.52055 0.2737 0.837865 0.072 Uiso 1 1 calc R U . . .
C103 C 0.5516(4) 0.1853(3) 0.7730(3) 0.0534(13) Uani 1 1 d . . . . .
H103 H 0.490311 0.1546 0.788416 0.064 Uiso 1 1 calc R U . . .
C104 C 0.6212(4) 0.1574(4) 0.7214(3) 0.0642(16) Uani 1 1 d . . . . .
H104 H 0.608957 0.107977 0.70129 0.077 Uiso 1 1 calc R U . . .
C105 C 0.7103(4) 0.2047(3) 0.7000(2) 0.0470(11) Uani 1 1 d . . . . .
H105 H 0.759976 0.187548 0.664731 0.056 Uiso 1 1 calc R U . . .
F1 F 0.8083(4) 0.3183(3) 0.7098(2) 0.0980(13) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 118.5(3) . . ?
C6 C1 N1 122.8(3) . . ?
C2 C1 N1 118.7(3) . . ?
C3 C2 C1 120.2(4) . . ?
C4 C3 C2 120.4(4) . . ?
C5 C4 C3 119.4(4) . . ?
C4 C5 C6 121.0(4) . . ?
C1 C6 C5 120.5(4) . . ?
C15 C11 C12 107.6(3) . . ?
C15 C11 C16 126.1(4) . . ?
C12 C11 C16 125.7(4) . . ?
C15 C11 Cr1 72.8(2) . . ?
C12 C11 Cr1 71.2(2) . . ?
C16 C11 Cr1 128.0(3) . . ?
C13 C12 C11 108.1(3) . . ?
C13 C12 C17 125.8(4) . . ?
C11 C12 C17 126.0(4) . . ?
C13 C12 Cr1 71.0(2) . . ?
C11 C12 Cr1 71.8(2) . . ?
C17 C12 Cr1 125.2(3) . . ?
C12 C13 C14 107.7(3) . . ?
C12 C13 C18 126.0(4) . . ?
C14 C13 C18 126.2(4) . . ?
C12 C13 Cr1 72.1(2) . . ?
C14 C13 Cr1 72.8(2) . . ?
C18 C13 Cr1 122.6(3) . . ?
C15 C14 C13 108.2(3) . . ?
C15 C14 C19 126.1(4) . . ?
C13 C14 C19 125.6(4) . . ?
C15 C14 Cr1 72.6(2) . . ?
C13 C14 Cr1 70.2(2) . . ?
C19 C14 Cr1 125.6(3) . . ?
C14 C15 C11 108.3(3) . . ?
C14 C15 C20 125.5(4) . . ?
C11 C15 C20 125.9(4) . . ?
C14 C15 Cr1 71.2(2) . . ?
C11 C15 Cr1 70.6(2) . . ?
C20 C15 Cr1 129.2(3) . . ?
N1 Cr1 N1 88.19(12) . 5_666 ?
N1 Cr1 C13 110.84(13) . . ?
N1 Cr1 C13 160.25(13) 5_666 . ?
N1 Cr1 C12 89.43(13) . . ?
N1 Cr1 C12 143.81(14) 5_666 . ?
C13 Cr1 C12 36.90(14) . . ?
N1 Cr1 C11 104.46(13) . . ?
N1 Cr1 C11 109.53(13) 5_666 . ?
C13 Cr1 C11 61.80(14) . . ?
C12 Cr1 C11 37.01(14) . . ?
N1 Cr1 C14 147.55(13) . . ?
N1 Cr1 C14 123.45(13) 5_666 . ?
C13 Cr1 C14 37.02(14) . . ?
C12 Cr1 C14 61.24(14) . . ?
C11 Cr1 C14 61.08(13) . . ?
N1 Cr1 C15 140.79(14) . . ?
N1 Cr1 C15 100.81(13) 5_666 . ?
C13 Cr1 C15 61.25(14) . . ?
C12 Cr1 C15 61.05(14) . . ?
C11 Cr1 C15 36.53(14) . . ?
C14 Cr1 C15 36.16(14) . . ?
N1 Cr1 Cl1 100.30(10) . . ?
N1 Cr1 Cl1 87.47(10) 5_666 . ?
C13 Cr1 Cl1 93.94(10) . . ?
C12 Cr1 Cl1 128.40(10) . . ?
C11 Cr1 Cl1 150.15(10) . . ?
C14 Cr1 Cl1 89.11(10) . . ?
C15 Cr1 Cl1 118.02(10) . . ?
N1 Cr1 Cr1 44.20(9) . 5_666 ?
N1 Cr1 Cr1 44.00(9) 5_666 5_666 ?
C13 Cr1 Cr1 154.65(10) . 5_666 ?
C12 Cr1 Cr1 123.78(10) . 5_666 ?
C11 Cr1 Cr1 114.00(10) . 5_666 ?
C14 Cr1 Cr1 166.15(11) . 5_666 ?
C15 Cr1 Cr1 132.01(10) . 5_666 ?
Cl1 Cr1 Cr1 95.37(3) . 5_666 ?
C1 N1 Cr1 128.3(3) . . ?
C1 N1 Cr1 126.3(2) . 5_666 ?
Cr1 N1 Cr1 91.81(12) . 5_666 ?
F1 C100 C105 119.2(5) . . ?
F1 C100 C101 117.8(5) . . ?
C105 C100 C101 123.0(5) . . ?
C100 C101 C102 116.7(5) . . ?
C103 C102 C101 121.6(5) . . ?
C102 C103 C104 121.3(6) . . ?
C103 C104 C105 117.6(6) . . ?
C100 C105 C104 119.8(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.383(5) . ?
C1 C2 1.401(5) . ?
C1 N1 1.423(5) . ?
C2 C3 1.390(6) . ?
C3 C4 1.379(7) . ?
C4 C5 1.371(6) . ?
C5 C6 1.387(6) . ?
C11 C15 1.420(5) . ?
C11 C12 1.426(5) . ?
C11 C16 1.495(5) . ?
C11 Cr1 2.251(4) . ?
C12 C13 1.415(5) . ?
C12 C17 1.505(5) . ?
C12 Cr1 2.243(4) . ?
C13 C14 1.426(5) . ?
C13 C18 1.496(5) . ?
C13 Cr1 2.228(4) . ?
C14 C15 1.409(5) . ?
C14 C19 1.503(5) . ?
C14 Cr1 2.261(4) . ?
C15 C20 1.502(5) . ?
C15 Cr1 2.279(4) . ?
Cl1 Cr1 2.3453(10) . ?
Cr1 N1 2.069(3) . ?
Cr1 N1 2.077(3) 5_666 ?
Cr1 Cr1 2.9776(11) 5_666 ?
C100 F1 1.292(6) . ?
C100 C105 1.364(7) . ?
C100 C101 1.378(7) . ?
C101 C102 1.382(8) . ?
C102 C103 1.369(8) . ?
C103 C104 1.385(8) . ?
C104 C105 1.402(7) . ?
