Forays into rhodium macrocyclic chemistry stabilized by a P<sub>2</sub>N<sub>2</sub> donor set. Activation of dihydrogen and benzene.
Yeo, Alyssa; Sanz, Corey A.; Fryzuk, Michael D.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 899–907; doi:10.1039/d0dt03688a

data_7705988
_publ_section_title
;
 Forays into rhodium macrocyclic chemistry stabilized by a
 P<sub>2</sub>N<sub>2</sub> donor set. Activation of dihydrogen and
 benzene.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              899
_journal_page_last               907
_journal_paper_doi               10.1039/d0dt03688a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 H45 N2 P2 Rh Si4'
_chemical_formula_sum            'C24 H45 N2 P2 Rh Si4'
_chemical_formula_weight         638.83
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-24 deposited with the CCDC.	2020-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.293(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1347(8)
_cell_length_b                   10.0758(5)
_cell_length_c                   20.3672(10)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      30.04
_cell_volume                     3092.6(3)
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_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f 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  0.0269
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
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_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.827
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         9055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.4864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8236
_reflns_number_total             9055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03688a2.cif
_cod_data_source_block           mf1376
_cod_depositor_comments
'Adding full bibliography for 7705986--7705991.cif.'
_cod_database_code               7705988
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.692
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C19(H19A,H19B), C24(H24A,H24B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C14(H14), C5(H5), C18(H18), C4(H4), C3(H3), C15(H15),
 C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C10(H10A,H10B,
 H10C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              68186
_olex2_submission_special_instructions 'No special instructions were received'