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_7705986
_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         '2(C26 H45 Li N2 O P2 Rh Si4), C6 H14'
_chemical_formula_sum            'C58 H104 Li2 N4 O2 P4 Rh2 Si8'
_chemical_formula_weight         1457.75
_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
_audit_creation_date             2020-03-03
_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                101.806(7)
_cell_angle_beta                 108.701(5)
_cell_angle_gamma                90.185(7)
_cell_formula_units_Z            2
_cell_length_a                   13.1434(14)
_cell_length_b                   15.766(2)
_cell_length_c                   19.777(2)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.518
_cell_measurement_theta_min      2.433
_cell_volume                     3789.2(8)
_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)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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_unetI/netI     0.0950
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.692
_diffrn_reflns_theta_min         2.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 93347 reflections, Rint = 0.1029
 (29896 with I > 3sig(I), Rint = 0.0721)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.789
_refine_diff_density_min         -2.150
_refine_diff_density_rms         0.172
_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     738
_refine_ls_number_reflns         22984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0828P)^2^+4.2298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16311
_reflns_number_total             22984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03688a2.cif
_cod_data_source_block           mf1441_4-new
_cod_depositor_comments
'Adding full bibliography for 7705986--7705991.cif.'
_cod_original_cell_volume        3789.4(8)
_cod_database_code               7705986
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5023(11)
 0.4977(11)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C19(H19C,H19D), C19A(H19A,H19B), C12(H12C,H12D), C26(H26C,
 H26D), C7(H7A,H7B), C26A(H26A,H26B), C9A(H9AA,H9AB), C25A(H25A,H25B), C25(H25C,
 H25D), C24(H24C,H24D), C7A(H7AA,H7AB), C11(H11D,H11E), C30(H30A,H30B),
 C29(H29A,H29B), C24A(H24A,H24B), C28(H28A,H28B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C4(H4), C3(H3), C18A(H18A), C6(H6), C2(H2), C14A(H14A),
 C18(H18), C3A(H3A), C15(H15), C5A(H5A), C17A(H17A), C6A(H6A), C2A(H2A),
 C16A(H16A), C15A(H15A), C4A(H4A), C5(H5), C16(H16)
3.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C21(H21D,H21E,H21F), C21A(H21A,H21B,H21C), C10(H10D,
 H10E,H10F), C10A(H10A,H10B,H10C), C20A(H20A,H20B,H20C), C8A(H8AA,H8AB,H8AC),
 C8(H8A,H8B,H8C), C23A(H23A,H23B,H23C), C22(H22D,H22E,H22F), C23(H23D,H23E,
 H23F), C20(H20D,H20E,H20F), C22A(H22A,H22B,H22C), C27(H27A,H27B,H27C),
 C32(H32A,H32B,H32C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              91993
_olex2_submission_special_instructions 'No special instructions were received'