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_7720083
_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         'C36 H42 N5 Rh, C3.5 H4'
_chemical_formula_sum            'C39.5 H46 N5 Rh'
_chemical_formula_weight         693.72
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-13
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2025-12-13 deposited with the CCDC.	2026-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.732(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9045(8)
_cell_length_b                   10.9709(5)
_cell_length_c                   21.0161(11)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.69
_cell_volume                     3424.8(3)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1593
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.548
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4280
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1139 before and 0.0888 after correction.
The Ratio of minimum to maximum transmission is 0.5740.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_recrystallization_method
'by diffusion of hexane into the toluene solution'
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7812
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0443P)^2^+6.9605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5380
_reflns_number_total             7812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00024j2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7720079--7720086.cif.'
_cod_original_formula_sum        'C39.50 H46 N5 Rh'
_cod_database_code               7720083
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C40) \\sim Ueq, : with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H39(0.5) C40(0.5) H40a(0.5) H40b(0.5) H40c(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C2(H2), C31(H31), C35(H35), C33(H33), C25(H25), C23(H23), C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C30(H30a,H30b), C34(H34a,H34b), C29(H29a,H29b), C19(H19a,
 H19b), C18(H18a,H18b), C32(H32a,H32b), C20(H20a,H20b), C36(H36a,H36b),
 C26(H26a,H26b), C24(H24a,H24b), C22(H22a,H22b)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C15(H15), C10(H10), C6(H6), C13(H13), C12(H12), C9(H9),
 C7(H7), C8(H8), C38(H38), C39(H39), C37(H37)
4.d Idealised Me refined as rotating group:
 C40(H40a,H40b,H40c)
;
_shelx_res_checksum              48253
_shelx_hkl_checksum              22580
_olex2_submission_original_sample_id mo_20251205f_0m
_olex2_submission_special_instructions 'No special instructions were received'