Twinned <i>versus</i> linked organometallics - bimetallic "half-baguette" pentalenide complexes of Rh(I).
Sanderson, Hugh J.; Kociok-Köhn, Gabriele; McMullin, Claire L.; Hintermair, Ulrich; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5881–5899; doi:10.1039/d3dt04325h

data_7715299
_publ_section_title
;
 Twinned <i>versus</i> linked organometallics - bimetallic "half-baguette"
 pentalenide complexes of Rh(I).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5881
_journal_page_last               5899
_journal_paper_doi               10.1039/d3dt04325h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H48 P4 Rh, C34 H22 O2 Rh, 4(C4 H8 O)'
_chemical_formula_sum            'C102 H102 O6 P4 Rh2'
_chemical_formula_weight         1753.53
_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_method           SHELXL-2018/3
_audit_update_record
;
2023-11-20 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                75.3403(16)
_cell_angle_beta                 87.2098(15)
_cell_angle_gamma                79.4900(15)
_cell_formula_units_Z            2
_cell_length_a                   13.9687(3)
_cell_length_b                   14.9315(3)
_cell_length_c                   22.8545(4)
_cell_measurement_reflns_used    20546
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.6550
_cell_measurement_theta_min      3.8140
_cell_volume                     4534.28(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47619
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.980
_diffrn_reflns_theta_min         3.784
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         17878
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+7.5938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15619
_reflns_number_total             17878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04325h2.cif
_cod_data_source_block           s22uh32
_cod_depositor_comments
'Adding full bibliography for 7715294--7715303.cif.'
_cod_database_code               7715299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.872
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_oxdiff_exptl_absorpt_empirical_full_max 1.328
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              24104