Enhancements in Catalytic Reactivity and Selectivity of Homobimetallic Complexes Containing Heteroditopic Ligands
Gatus, Mark; McBurney, Roy Thomas; Bhadbhade, Mohan; Messerle, Barbara A.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01294B

data_7043099
_publ_section_title
;
 Enhancements in Catalytic Reactivity and Selectivity of Homobimetallic
 Complexes Containing Heteroditopic Ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01294B
_journal_year                    2017
_chemical_formula_moiety         'C50 H64 Cl2 N6 O2 Rh2, C H2.8'
_chemical_formula_sum            'C51 H66.8 Cl2 N6 O2 Rh2'
_chemical_formula_weight         1072.62
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.018(3)
_cell_length_b                   25.511(5)
_cell_length_c                   27.991(6)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     10708(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68593
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.095
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       plate
_exptl_crystal_F_000             4438
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.833
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9436
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0581P)^2^+42.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7456
_reflns_number_total             9436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01294b2.cif
_cod_data_source_block           mark1_renamed
_cod_original_formula_sum        'C51 H66.80 Cl2 N6 O2 Rh2'
_cod_database_code               7043099
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.989
_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, All O(H) groups
2. Restrained distances
 C165-C166 \\sim C165-C164 \\sim C163-C162 \\sim C162-C161
 with sigma of 0.04
 C15-C2 \\sim C15-C165 \\sim C15-C163 \\sim C15-C166 \\sim C15-C164 \\sim
C15-C162 \\sim C15-C161
 with sigma of 0.02
 C15-C168 \\sim C15-C167 \\sim C15-C165 \\sim C15-C163 \\sim C15-C2 \\sim
C15-C161 \\sim C15-C164 ~
 C15-C166 \\sim C15-C162 \\sim C15-C169
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C162) = Uanis(C165) = Uanis(C168)
4. Rigid body (RIGU) restrains
 C0BA, C1BA, C9AA
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2, C15, C167, C168, C169, C163, C165, C164, C161, C162, C166
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C168, C165
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C167(0.3) H16D(0.3) H16E(0.3) H16F(0.3) C168(0.3) H16G(0.3)
 H16H(0.3) H16I(0.3) C169(0.3) H16A(0.3) H16B(0.3) H16C(0.3) C163(0.3)
 H1AA(0.3) H1AB(0.3) H1AC(0.3) C165(0.4) H4AA(0.4) H4AB(0.4) H4AC(0.4)
 C0BA(0.4) H0BA(0.4) H0BB(0.4) C1BA(0.2) H1BA(0.4) H1BB(0.4) C9AA(0.4)
 H9AA(0.4) H9AB(0.4) H9AC(0.4) C164(0.4) H3AA(0.4) H3AB(0.4) H3AC(0.4)
 C161(0.3) H0AA(0.3) H0AB(0.3) H0AC(0.3) C162(0.3) H2AA(0.3) H2AB(0.3)
 H2AC(0.3) C166(0.4) H5AA(0.4) H5AB(0.4) H5AC(0.4)
6.a Ternary CH refined with riding coordinates:
 C2'(H2'), C20(H20), C21(H21), C24(H24), C25(H25), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C33(H33A,
 H33B), C36(H36A,H36B), C37(H37A,H37B), C0BA(H0BA,H0BB), C1BA(H1BA,H1BB)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C1B(H1B), C1C(H1C), C3(H3), C3'(H3'), C3*(H3*), C4'(H4'), C4*(H4*),
 C5'(H5'), C5*(H5*), C6(H6), C8(H8)
6.d Idealised Me refined as rotating group:
 C1D(H1DA,H1DB,H1DC), C14A(H14D,H14E,H14F), C14B(H14A,H14B,H14C), C18A(H18G,
 H18H,H18I), C18B(H18A,H18B,H18C), C18C(H18D,H18E,H18F), C167(H16D,H16E,H16F),
 C168(H16G,H16H,H16I), C169(H16A,H16B,H16C), C163(H1AA,H1AB,H1AC), C165(H4AA,
 H4AB,H4AC), C9AA(H9AA,H9AB,H9AC), C164(H3AA,H3AB,H3AC), C161(H0AA,H0AB,H0AC),
 C162(H2AA,H2AB,H2AC), C166(H5AA,H5AB,H5AC)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'