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_7705991
_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         'C64 H104 Li2 N4 O2 P4 Rh2 Si8, 4(C6 H6)'
_chemical_formula_sum            'C88 H128 Li2 N4 O2 P4 Rh2 Si8'
_chemical_formula_weight         1842.24
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-16 deposited with the CCDC.	2020-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.810(7)
_cell_angle_beta                 94.411(7)
_cell_angle_gamma                103.071(6)
_cell_formula_units_Z            1
_cell_length_a                   11.3155(12)
_cell_length_b                   12.3073(13)
_cell_length_c                   17.4753(18)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    90
_cell_measurement_theta_max      36.575
_cell_measurement_theta_min      2.300
_cell_volume                     2345.9(4)
_computing_cell_refinement       'SAINT V8.40A (2016)'
_computing_data_reduction        'SAINT V8.40A (2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.692
_diffrn_reflns_theta_min         1.177
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1234 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9109. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       prisms
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         22948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0293
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19948
_reflns_number_total             22948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03688a2.cif
_cod_data_source_block           mf1442
_cod_depositor_comments
'Adding full bibliography for 7705986--7705991.cif.'
_cod_database_code               7705991
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.780
_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:
 C7(H7A,H7B), C12(H12A,H12B), C19(H19A,H19B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22B,H22C,H22A), C23(H23B,H23C,
 H23A)
;
_shelx_res_checksum              51391
_olex2_submission_special_instructions 'No special instructions were received'