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_7123242
_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         'C28 H27 N4 Rh'
_chemical_formula_sum            'C28 H27 N4 Rh'
_chemical_formula_weight         522.44
_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             2019-01-16
_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                88.376(3)
_cell_angle_beta                 78.045(3)
_cell_angle_gamma                82.826(3)
_cell_formula_units_Z            4
_cell_length_a                   8.6127(3)
_cell_length_b                   14.8452(5)
_cell_length_c                   20.5926(7)
_cell_measurement_reflns_used    3793
_cell_measurement_temperature    294
_cell_measurement_theta_max      23.4770
_cell_measurement_theta_min      3.7190
_cell_volume                     2555.63(15)
_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_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.809
_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    -38.00  61.00   0.75   59.33    --  -10.80  57.00  30.00  132
  2  \w    -78.00  12.00   0.75   59.33    --  -10.80 -57.00-120.00  120
  3  \w     34.00 100.00   0.75   59.33    --   12.36-178.00-120.00   88
;
_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      0.0047339000
_diffrn_orient_matrix_UB_12      -0.0420359000
_diffrn_orient_matrix_UB_13      -0.0162632000
_diffrn_orient_matrix_UB_21      0.0845093000
_diffrn_orient_matrix_UB_22      -0.0020324000
_diffrn_orient_matrix_UB_23      -0.0082626000
_diffrn_orient_matrix_UB_31      0.0053835000
_diffrn_orient_matrix_UB_32      -0.0234065000
_diffrn_orient_matrix_UB_33      0.0301146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17904
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.707
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.651
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0231P)^2^+0.1946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6327
_reflns_number_total             11736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01377f2.cif
_cod_data_source_block           4
_cod_database_code               7123242
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H27 N4 Rh'
_chemical_oxdiff_usercomment     YELLOW
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C4C(H4C), C5A(H5A), C5B(H5B), C5C(H5C), C6A(H6A),
 C6B(H6B), C6C(H6C), C4A*(H4A*), C4B*(H4B*), C4C*(H4C*), C5A*(H5A*), C5B*(H5B*),
  C5C*(H5C*), C6A*(H6A*), C6B*(H6B*), C6C*(H6C*)
2.b Idealised Me refined as rotating group:
 C8A(H8AD,H8AE,H8AF), C8B(H8BD,H8BE,H8BF), C8C(H8CD,H8CE,H8CF), C9A(H9AD,H9AE,
 H9AF), C9B(H9BD,H9BE,H9BF), C9C(H9CD,H9CE,H9CF), C8A*(H8AA,H8AB,H8AC), C8B*
 (H8BA,H8BB,H8BC), C8C*(H8CA,H8CB,H8CC), C9A*(H9AA,H9AB,H9AC), C9B*(H9BA,H9BB,
 H9BC), C9C*(H9CA,H9CB,H9CC)
;
_shelx_res_checksum              5999
_shelx_hkl_checksum              582
_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 1.144
_oxdiff_exptl_absorpt_empirical_full_min 0.715