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_7705987
_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         'C68 H120 Li2 N4 O2 P4 Rh2 Si8'
_chemical_formula_sum            'C68 H120 Li2 N4 O2 P4 Rh2 Si8'
_chemical_formula_weight         1593.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-24
_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                 92.872(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7614(5)
_cell_length_b                   22.3119(13)
_cell_length_c                   17.1063(8)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.29
_cell_measurement_theta_min      25.25
_cell_volume                     4102.2(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.972
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16275
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.314
_diffrn_reflns_theta_min         1.825
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.8971
_exptl_absorpt_correction_T_min  0.6689
_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    1.290
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0639P)^2^+0.5857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5134
_reflns_number_total             7270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03688a2.cif
_cod_data_source_block           mf1365
_cod_depositor_comments
'Adding full bibliography for 7705986--7705991.cif.'
_cod_database_code               7705987
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.846
_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(C29) = Uanis(C29A)
Uanis(C28) = Uanis(C28A)
Uanis(C27) = Uanis(C27A)
Uanis(C26) = Uanis(C26A)
Uanis(C25) = Uanis(C25A)
3. Others
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=FVAR(2)
 Fixed Sof: P2A(0.5) C30A(0.5) H30A(0.5) H30B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C22A(0.5) C21A(0.5) C31A(0.5) C32(0.5) C30(0.5) H30C(0.5) H30D(0.5)
 C23A(0.5) H23C(0.5) H23D(0.5) C32A(0.5) C31(0.5) C22(0.5) C21(0.5) C29(0.5)
 H29(0.5) C28(0.5) H28(0.5) C27(0.5) H27(0.5) C26(0.5) H26(0.5) C25(0.5)
 H25(0.5) C29A(0.5) H29A(0.5) C28A(0.5) H28A(0.5) C27A(0.5) H27A(0.5) C26A(0.5)
 H26A(0.5) C25A(0.5) H25A(0.5) P2(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C8(H8A,H8B), C3(H3A,H3B), C7(H7A,H7B), C4(H4A,
 H4B), C6(H6A,H6B), C5(H5A,H5B), C30A(H30A,H30B), C23(H23A,H23B), C34(H34A,
 H34B), C33(H33A,H33B), C30(H30C,H30D), C23A(H23C,H23D)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C29(H29), C28(H28),
 C27(H27), C26(H26), C25(H25), C29A(H29A), C28A(H28A), C27A(H27A), C26A(H26A),
 C25A(H25A)
4.d Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C24(C29,C28,C27,C26,C25)
4.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C19(H19A,H19B,
 H19C), C22A(H22A,H22B,H22C), C21A(H21A,H21B,H21C), C31A(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F), C31(H31D,H31E,H31F), C22(H22D,H22E,
 H22F), C21(H21D,H21E,H21F)
;
_shelx_res_checksum              62322
_olex2_submission_special_instructions 'No special instructions were received'