d8···d10 RhI···AuI Interactions in Rh 2,6-Xylylisocyanide Complexes with [Au(CN)2]‒: Bond Analysis and Crystal Effects
Conejo-Rodríguez, Verónica; Peñas-Defrutos, Marconi N.; Espinet, Pablo; Chemical Communications  (2019) –; doi:10.1039/C9CC01377F

data_7123244
_publ_section_title
;
 d8&#x00B7;&#x00B7;&#x00B7;d10 RhI&#x00B7;&#x00B7;&#x00B7;AuI Interactions
 in Rh 2,6-Xylylisocyanide Complexes with [Au(CN)2]--: Bond Analysis and
 Crystal Effects
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01377F
_journal_year                    2019
_chemical_formula_moiety         'C38 H36 Au N6 Rh, C H Cl3'
_chemical_formula_sum            'C39 H37 Au Cl3 N6 Rh'
_chemical_formula_weight         995.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-30 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                110.029(6)
_cell_angle_beta                 90.594(5)
_cell_angle_gamma                99.495(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6734(5)
_cell_length_b                   15.7599(12)
_cell_length_c                   17.8463(10)
_cell_measurement_reflns_used    4560
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      26.8570
_cell_measurement_theta_min      3.4450
_cell_volume                     1994.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  63.00   1.00   14.61    --  -10.64  57.00-150.00   98
  2  \w    -76.00  18.00   1.00   14.61    --  -10.64 -57.00  60.00   94
  3  \w     34.00  99.00   1.00   14.61    --   12.20-178.00  60.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0869130000
_diffrn_orient_matrix_UB_12      0.0260282000
_diffrn_orient_matrix_UB_13      0.0057251000
_diffrn_orient_matrix_UB_21      -0.0043371000
_diffrn_orient_matrix_UB_22      0.0128791000
_diffrn_orient_matrix_UB_23      0.0420187000
_diffrn_orient_matrix_UB_31      0.0354509000
_diffrn_orient_matrix_UB_32      -0.0390862000
_diffrn_orient_matrix_UB_33      -0.0007838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13755
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.608
_diffrn_reflns_theta_min         3.419
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.323
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.440
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0400P)^2^+0.4738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6718
_reflns_number_total             9062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01377f2.cif
_cod_data_source_block           2a
_cod_database_code               7123244
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C38 H36 Au N6 Rh'
_chemical_oxdiff_usercomment     orange
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.247
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Sof(H50A)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=1-FVAR(1)
 Sof(H50)=Sof(Cl1Z)=Sof(Cl2Z)=Sof(Cl3Z)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C50(H50), C50(H50A)
3.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C4C(H4C), C4D(H4D), C5A(H5A), C5B(H5B), C5C(H5C),
 C5D(H5D), C6A(H6A), C6B(H6B), C6C(H6C), C6D(H6D)
3.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BC,H8BB), C8C(H8CA,H8CB,H8CC), C8D(H8DA,H8DB,
 H8DC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC), C9D(H9DA,
 H9DB,H9DC)
;
_shelx_res_checksum              63302
_shelx_hkl_checksum              93659
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.732