Heterobimetallic complexes stabilized by the P2N2 macrocyclic ligand system: synthesis and reactivity of a rhodium–copper system that activates molecular hydrogen
Xie, Siyuan L.; Sanz, Corey A.; Fryzuk, Michael D.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03129E

data_7708819
_publ_section_title
;
 Heterobimetallic complexes stabilized by the P2N2 macrocyclic ligand
 system: synthesis and reactivity of a rhodium--copper system that
 activates molecular hydrogen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03129E
_journal_year                    2021
_chemical_formula_moiety         'C32 H56 Cu N2 P2 Rh Si4'
_chemical_formula_sum            'C32 H56 Cu N2 P2 Rh Si4'
_chemical_formula_weight         809.53
_chemical_name_systematic        Rh(COE)[P2N2]Cu
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-03 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.314(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9598(7)
_cell_length_b                   13.5924(6)
_cell_length_c                   18.3198(8)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    90
_cell_measurement_theta_max      59.15
_cell_measurement_theta_min      2.834
_cell_volume                     3882.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43620
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        59.368
_diffrn_reflns_theta_max         59.368
_diffrn_reflns_theta_min         2.834
_exptl_absorpt_coefficient_mu    6.250
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1076 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.6583.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5623
_refine_ls_number_restraints     896
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0537P)^2^+6.7052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4348
_reflns_number_total             5623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03129e2.cif
_cod_data_source_block           mf1444
_cod_database_code               7708819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.368
_olex2_refinement_description
;
1. Restrained distances
 C27A-C26A
 1.54 with sigma of 0.02
 C25A-C26A
 1.54 with sigma of 0.02
 C30A-C31A
 1.54 with sigma of 0.02
 C29A-C30A
 1.54 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27C)=
 Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=
 Sof(H32A)=1-FVAR(1)
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C25A(H25A), C32(H32), C32A(H32A)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C26(H26A,H26B), C26A(H26C,
 H26D), C27(H27A,H27B), C27A(H27C,H27D), C28(H28A,H28B), C28A(H28C,H28D),
 C29(H29A,H29B), C29A(H29C,H29D), C30(H30A,H30B), C30A(H30C,H30D), C31(H31A,
 H31B), C31A(H31C,H31D)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              87281
_shelx_hkl_checksum              57457
_olex2_submission_special_instructions 'No special instructions were received'