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_7708820
_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         'C48 H92 Cu2 N4 P4 Rh2 Si8, 2(C7 H8)'
_chemical_formula_sum            'C62 H108 Cu2 N4 P4 Rh2 Si8'
_chemical_formula_weight         1591.02
_chemical_name_systematic        ([P2N2H]Rh(H)(\m-H)2Cu)2
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 128.4150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.949(3)
_cell_length_b                   13.5303(10)
_cell_length_c                   21.6795(17)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      30.523
_cell_measurement_theta_min      2.514
_cell_volume                     7802.6(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         1.531
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0512 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.9097.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         11955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+7.1092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9335
_reflns_number_total             11955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03129e2.cif
_cod_data_source_block           mf1451
_cod_original_cell_volume        7802.5(10)
_cod_database_code               7708820
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11A(0.03) H11B(0.03) H9A(0.029) H9B(0.029) H10A(0.031)
 H10B(0.031) H12A(0.032) H12B(0.032) H18(0.039) H17(0.051) H16(0.058)
 H15(0.056) H14(0.04) H24(0.037) H23(0.054) H22(0.066) H21(0.068) H20(0.05)
 H4A(0.061) H4B(0.061) H4C(0.061) H3A(0.055) H3B(0.055) H3C(0.055) H2A(0.054)
 H2B(0.054) H2C(0.054) H1A(0.057) H1B(0.057) H1C(0.057) H8A(0.055) H8B(0.055)
 H8C(0.055) H7A(0.062) H7B(0.062) H7C(0.062) H6A(0.072) H6B(0.072) H6C(0.072)
 H5A(0.06) H5B(0.06) H5C(0.06) H30A(0.091) H30B(0.091) H30C(0.091) H25(0.061)
 H26(0.084) H27(0.084) H28(0.079) H29(0.052) H32A(0.108) H32B(0.108)
 H32C(0.108) H34(0.043) H35(0.055) H36(0.053) H37(0.062) H38(0.049)
 Fixed X: H11A(0.6982) H11B(0.698962) H9A(0.684631) H9B(0.666988)
 H10A(0.56544) H10B(0.620387) H12A(0.692374) H12B(0.671345) H18(0.675867)
 H17(0.651202) H16(0.567938) H15(0.509432) H14(0.533936) H24(0.516535)
 H23(0.466435) H22(0.477933) H21(0.537641) H20(0.587222) H4A(0.707387)
 H4B(0.718848) H4C(0.742469) H3A(0.57399) H3B(0.6109) H3C(0.59841)
 H2A(0.750027) H2B(0.754293) H2C(0.743156) H1A(0.655225) H1B(0.658262)
 H1C(0.608806) H8A(0.70811) H8B(0.707195) H8C(0.702765) H7A(0.575106)
 H7B(0.626265) H7C(0.624169) H6A(0.688868) H6B(0.66734) H6C(0.639921)
 H5A(0.586853) H5B(0.552584) H5C(0.548178) H30A(0.733792) H30B(0.692705)
 H30C(0.74183) H25(0.74286) H26(0.705056) H27(0.630964) H28(0.594956)
 H29(0.632874) H32A(0.632572) H32B(0.689223) H32C(0.652558) H34(0.618678)
 H35(0.637558) H36(0.703723) H37(0.754073) H38(0.732126)
 Fixed Y: H11A(0.587743) H11B(0.69022) H9A(0.860734) H9B(0.970668)
 H10A(0.908386) H10B(0.949755) H12A(0.591124) H12B(0.484899) H18(0.423705)
 H17(0.284462) H16(0.262473) H15(0.381743) H14(0.522987) H24(0.879409)
 H23(1.004653) H22(1.165472) H21(1.200732) H20(1.07603) H4A(0.742583)
 H4B(0.634635) H4C(0.724903) H3A(0.65179) H3B(0.573577) H3C(0.670469)
 H2A(0.849764) H2B(0.964814) H2C(0.917831) H1A(1.052193) H1B(1.092629)
 H1C(1.042157) H8A(0.732834) H8B(0.84586) H8C(0.767282) H7A(0.805688)
 H7B(0.862076) H7C(0.747301) H6A(0.572872) H6B(0.46504) H6C(0.549681)
 H5A(0.399245) H5B(0.469004) H5C(0.469423) H30A(0.878995) H30B(0.799178)
 H30C(0.769233) H25(0.94208) H26(0.973811) H27(0.894089) H28(0.782839)
 H29(0.751281) H32A(0.969231) H32B(0.96353) H32C(0.876652) H34(0.77817)
 H35(0.70526) H36(0.763217) H37(0.888264) H38(0.959209)
 Fixed Z: H11A(0.770351) H11B(0.804164) H9A(0.848538) H9B(0.834861)
 H10A(0.841856) H10B(0.88897) H12A(0.902457) H12B(0.867811) H18(0.767049)
 H17(0.691055) H16(0.583001) H15(0.551972) H14(0.628213) H24(0.607993)
 H23(0.520217) H22(0.564498) H21(0.696467) H20(0.784569) H4A(0.628574)
 H4B(0.661915) H4C(0.719756) H3A(0.573205) H3B(0.580917) H3C(0.532195)
 H2A(0.809696) H2B(0.820612) H2C(0.745104) H1A(0.650213) H1B(0.72083)
 H1C(0.649159) H8A(1.02827) H8B(1.011512) H8C(0.954341) H7A(0.970758)
 H7B(1.027636) H7C(1.035148) H6A(1.030526) H6B(1.011017) H6C(1.020487)
 H5A(0.859838) H5B(0.786928) H5C(0.854748) H30A(0.400627) H30B(0.346293)
 H30C(0.4294) H25(0.515987) H26(0.572942) H27(0.527403) H28(0.424015)
 H29(0.367183) H32A(0.493923) H32B(0.568664) H32C(0.549274) H34(0.427945)
 H35(0.349176) H36(0.357044) H37(0.446319) H38(0.51716)
;
_shelx_res_checksum              1169
_shelx_hkl_checksum              1837
_olex2_submission_special_instructions 'No special instructions were received'