Unquenched orbital angular momentum in quasi-linear two-coordinate transition metal complexes featuring sterically bulky carbazole ligands.
Noor, Sadia; Stegman, Samantha; Palmer, Jacob B.; Dolinar, Brian S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11495–11499; doi:10.1039/d5dt00782h

data_7718948
_publ_section_title
;
 Unquenched orbital angular momentum in quasi-linear two-coordinate
 transition metal complexes featuring sterically bulky carbazole ligands.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11495
_journal_page_last               11499
_journal_paper_doi               10.1039/d5dt00782h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C92 H88 Fe N2'
_chemical_formula_sum            'C92 H88 Fe N2'
_chemical_formula_weight         1277.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-03-19 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.610(3)
_cell_angle_beta                 101.715(2)
_cell_angle_gamma                95.375(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9927(9)
_cell_length_b                   12.5791(10)
_cell_length_c                   24.7232(15)
_cell_measurement_reflns_used    1733
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.25
_cell_volume                     3581.1(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'PHOTON II CMOS area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Triumph Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23463
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.738
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'sealed tube'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0724 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.8935.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         13481
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1281P)^2^+5.5843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2558
_refine_ls_wR_factor_ref         0.2807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7871
_reflns_number_total             13481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00782h2.cif
_cod_data_source_block           2-Fe
_cod_depositor_comments
'Adding full bibliography for 7718947--7718950.cif.'
_cod_original_cell_volume        3581.0(4)
_cod_database_code               7718948
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C76 \\sim C77 \\sim C78 \\sim C79 \\sim C76A \\sim C77A \\sim C78A \\sim C79A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C26A \\sim C27A \\sim C28A \\sim C29A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
3. Same fragment restrains
{C26A, C27A, C28A, C29A} sigma for 1-2: 0.01, 1-3: 0.02
{C76, C77, C78, C79} sigma for 1-2: 0.01, 1-3: 0.02
{C76A, C77A, C78A, C79A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C26, C27, C28, C29}
4. Others
 Sof(C26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(C76A)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78A)=Sof(H78D)=
 Sof(H78E)=Sof(H78F)=Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=1-FVAR(2)
 Sof(C76)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)=
 Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C34(H34), C59(H59), C80(H80)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C36(H36), C37(H37),
  C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C49(H49), C51(H51), C54(H54), C56(H56), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90),
  C91(H91), C92(H92)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C79(H79A,H79B,H79C), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C29A(H29D,
 H29E,H29F), C77A(H77D,H77E,H77F), C78A(H78D,H78E,H78F), C79A(H79D,H79E,H79F)
;
_shelx_res_checksum              54657
_shelx_hkl_checksum              24599
_olex2_submission_special_instructions 'No special instructions were received'