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_7705990
_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         'C40 H66 N2 P2 Rh2 Si4'
_chemical_formula_sum            'C40 H66 N2 P2 Rh2 Si4'
_chemical_formula_weight         955.06
_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             2020-01-13
_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                 100.362(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3474(6)
_cell_length_b                   16.4155(12)
_cell_length_c                   25.8521(18)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      2.29
_cell_measurement_theta_min      25.02
_cell_volume                     4319.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      90.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31583
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         1.476
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8418
_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    1.469
_exptl_crystal_description       shard
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0354P)^2^+5.4429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5845
_reflns_number_total             7645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03688a2.cif
_cod_data_source_block           mf1324
_cod_depositor_comments
'Adding full bibliography for 7705986--7705991.cif.'
_cod_database_code               7705990
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.851
_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 Ternary CH refined with riding coordinates:
 C38(H38), C30(H30), C29(H29), C26(H26), C37(H37), C25(H25), C34(H34), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C12(H12A,H12B), C19(H19A,H19B), C7(H7A,H7B), C32(H32A,H32B),
 C31(H31A,H31B), C36(H36A,H36B), C39(H39A,H39B), C28(H28A,H28B), C40(H40A,H40B),
  C27(H27A,H27B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C3(H3), C18(H18), C2(H2), C17(H17), C6(H6),
 C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C10(H10A,H10B,
 H10C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C8(H8A,H8B,
 H8C)
;
_shelx_res_checksum              11983
_olex2_submission_special_instructions 'No special instructions were received'