Highly Versatile Heteroditopic Ligand Scaffolds for Accommodating Group 8, 9 & 11 Heterobimetallic Complexes
Gatus, Mark; Bhadbhade, Mohan; Messerle, Barbara A.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02854G

data_7044420
_publ_section_title
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 Highly Versatile Heteroditopic Ligand Scaffolds for Accommodating Group
 8, 9 &amp; 11 Heterobimetallic Complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02854G
_journal_year                    2017
_chemical_formula_moiety         'C50 H64 Cl Ir N6 O Rh, C24 H20 B'
_chemical_formula_sum            'C74 H84 B Cl Ir N6 O Rh'
_chemical_formula_weight         1414.93
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2014-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2016-12-16 deposited with the CCDC.
2017-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.72(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.462(4)
_cell_length_b                   23.367(5)
_cell_length_c                   16.797(3)
_cell_volume                     7388(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_measured_fraction_theta_full 0.9763
_diffrn_measured_fraction_theta_max 0.9763
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            155483
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    2.102
_exptl_crystal_density_diffrn    1.2720
_exptl_crystal_F_000             2879.7948
_refine_diff_density_max         1.6566
_refine_diff_density_min         -1.7778
_refine_diff_density_rms         0.1188
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             13.3385
_refine_ls_goodness_of_fit_ref   0.8077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    142
_refine_ls_number_parameters     774
_refine_ls_number_reflns         12701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8077
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+17.1794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                11171
_reflns_number_total             12701
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02854g2.cif
_cod_data_source_block           Mark2_renamed
_cod_database_code               7044420
_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:
 C20(H20), C21(H21), C24(H24), C25(H25), C30(H30), C31(H31), C34(H34),
 C35(H35), C2'(H2')
2.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C26(H26a,H26b), C27(H27a,H27b), C32(H32a,
 H32b), C33(H33a,H33b), C36(H36a,H36b), C37(H37a,H37b)
2.c Aromatic/amide H refined with riding coordinates:
 C3'(H3'), C4'(H4'), C5'(H5'), C3*(H3*), C4*(H4*), C5*(H5*), C1(H1), C3(H3),
 C6(H6), C8(H8), C1B(H1B), C1C(H1C), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54),
  C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
2.d Idealised Me refined as rotating group:
 C1D(H1Da,H1Db,H1Dc), C14A(H14a,H14b,H14c), C14B(H14d,H14e,H14f), C16A(H16a,
 H16b,H16c), C16B(H16d,H16e,H16f), C16C(H16g,H16h,H16i), C18A(H18a,H18b,H18c),
 C18B(H18d,H18e,H18f), C18C(H18g,H18h,H18i)
;