Half-sandwich η<sup>5</sup>-pyrrolyl rhodium(I) complexes with alkene coordination: synthesis and reactivity exploration.
Yan, Jiayu; Sun, Jian; Zhou, Shuangliu; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3682–3686; doi:10.1039/d6dt00024j

data_7720085
_publ_section_title
;
 Half-sandwich &#x3b7;<sup>5</sup>-pyrrolyl rhodium(I) complexes with
 alkene coordination: synthesis and reactivity exploration.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3682
_journal_page_last               3686
_journal_paper_doi               10.1039/d6dt00024j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C33 H35 N4 Rh'
_chemical_formula_sum            'C33 H35 N4 Rh'
_chemical_formula_weight         590.56
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-17
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2026-01-20 deposited with the CCDC.	2026-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                87.727(4)
_cell_angle_beta                 89.490(5)
_cell_angle_gamma                83.562(5)
_cell_formula_units_Z            4
_cell_length_a                   7.6385(11)
_cell_length_b                   19.358(3)
_cell_length_c                   20.350(3)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.777
_cell_measurement_theta_min      2.773
_cell_volume                     2987.7(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70278
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.650
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.7024.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_recrystallization_method 'from the saturated THF/hexane solution'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.897
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         13588
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0957
_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^)+(0.0842P)^2^+27.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2596
_refine_ls_wR_factor_ref         0.2821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8947
_reflns_number_total             13588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00024j2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7720079--7720086.cif.'
_cod_database_code               7720085
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.860
_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. Rigid bond restraints
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C11, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C14, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C27, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C34, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C39, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C46, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C43, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C47, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C42, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C53, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C62, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C61, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C51, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C51, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C10(H10), C11(H11), C12(H12), C19(H19), C20(H20), C21(H21),
 C28(H28), C29(H29), C30(H30), C35(H35), C36(H36), C43(H43), C44(H44), C45(H45),
  C52(H52), C53(H53), C54(H54), C61(H61), C62(H62), C63(H63)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C)
;
_shelx_res_checksum              92424
_shelx_hkl_checksum              15474
_olex2_submission_original_sample_id mo_20230915f_0m
_olex2_submission_special_instructions 'No special instructions were received'