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_7044419
_publ_section_title
;
 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         'C42 H51 Au Cl I N6 O Rh'
_chemical_formula_sum            'C42 H51 Au Cl I N6 O Rh'
_chemical_formula_weight         1118.14
_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_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.356(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.393(4)
_cell_length_b                   15.0582(13)
_cell_length_c                   21.186(2)
_cell_measurement_reflns_used    9896
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.28
_cell_volume                     10587.7(19)
_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_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83515
_diffrn_reflns_theta_full        26.3716
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.8459.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.4029
_exptl_crystal_F_000             4351.9093
_refine_diff_density_max         3.0536
_refine_diff_density_min         -3.0387
_refine_diff_density_rms         0.1940
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             16.5937
_refine_ls_goodness_of_fit_ref   1.0424
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    102
_refine_ls_number_parameters     528
_refine_ls_number_reflns         10817
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.0411
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          3.3092
_refine_ls_shift/su_mean         0.0408
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+60.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              41
_reflns_limit_h_min              -41
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                7751
_reflns_number_total             10817
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02854g2.cif
_cod_data_source_block           Mark_03Sept13_renamed
_cod_original_cell_volume        10587.4(18)
_cod_database_code               7044419
_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. Shared sites
{N5, N00B}
{C2, C002}
3. Restrained distances
 C6-C0AA \\sim C1-C17 \\sim C13-C11
 with sigma of 0.02
 C6-C1 \\sim C1-C13
 with sigma of 0.02
 C17-C00X \\sim C00X-C13
 with sigma of 0.02
 C1-C13 \\sim C1-C6 \\sim C17-C0AA \\sim C17-C11 \\sim C0AA-C11
 with sigma of 0.04
 C00X-C00I \\sim C00X-C1 \\sim C00X-C17 \\sim C00X-C0AA \\sim C00X-C13 \\sim
C00X-C6 \\sim C00X-C11
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C13 \\sim C6 \\sim C1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C17 \\sim C11 \\sim C0AA: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C00X \\sim C13: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(N5) = Uanis(N00B)
Uanis(C2) = Uanis(C002)
5. Others
 Fixed Sof: N00B(0.5) N01I(0.5) C14(0.5) H14(0.5) C4(0.5) H4(0.5) C1(0.6)
 H1a(0.6) H1b(0.6) H1c(0.6) C17(0.4) H17a(0.4) H17b(0.4) H17c(0.4) C0AA(0.4)
 H0Aa(0.4) H0Ab(0.4) H0Ac(0.4) C13(0.6) H13a(0.6) H13b(0.6) H13c(0.6) C6(0.6)
 H6a(0.6) H6b(0.6) H6c(0.6) C11(0.4) H11a(0.4) H11b(0.4) H11c(0.4) N4(0.5)
 C5(0.5) H5(0.5) C7(0.5) H7(0.5) N5(0.5) C2(0.5) H2(0.5) C002(0.5) H002(0.5)
6.a Ternary CH refined with riding coordinates:
 C00G(H00G), C00J(H00J), C00Y(H00Y), C010(H010)
6.b Secondary CH2 refined with riding coordinates:
 C011(H01a,H01b), C012(H01c,H01d), C018(H01k,H01l), C01A(H01m,H01n)
6.c Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00H(H00H), C00M(H00M), C00P(H00P), C00U(H00U),
 C00V(H00V), C014(H014), C015(H015), C14(H14), C4(H4), C5(H5), C7(H7), C2(H2),
 C002(H002)
6.d Idealised Me refined as rotating group:
 C00R(H00a,H00b,H00c), C00S(H00f,H00i,H00k), C016(H01e,H01f,H01g), C017(H01h,
 H01i,H01j), C01D(H01o,H01p,H01q), C01G(H01r,H01s,H01t), C1(H1a,H1b,H1c),
 C17(H17a,H17b,H17c), C0AA(H0Aa,H0Ab,H0Ac), C13(H13a,H13b,H13c), C6(H6a,H6b,
 H6c), C11(H11a,H11b,H11c)
;