Probing the Effect of Six-Membered N-Heterocyclic Carbene-6-Mes-on the Synthesis, Structure and Reactivity of Me2MOR(NHC) (M = Ga, In) Complexes
Cybularczyk-Cecotka, M.; Dabrowska, A.M.; Gunka, P.A.; Horeglad, P.; Inorganics 6 (2018) 28–; doi:10.3390/inorganics6010028

data_1556594
_publ_section_title
;
 Probing the Effect of Six-Membered N-Heterocyclic Carbene-6-Mes-on the
 Synthesis, Structure and Reactivity of Me2MOR(NHC) (M = Ga, In) Complexes
;
_journal_name_full               Inorganics
_journal_page_first              28
_journal_paper_doi               10.3390/inorganics6010028
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C25 H37 In N2'
_chemical_formula_sum            'C25 H37 In N2'
_chemical_formula_weight         480.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 106.868(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5680(3)
_cell_length_b                   16.9878(4)
_cell_length_c                   16.0384(5)
_cell_measurement_reflns_used    11913
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.4380
_cell_measurement_theta_min      4.0800
_cell_volume                     2494.71(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -27.00  -1.00   1.00    6.50    --  -12.96 -38.00 -30.00   26
  2  \w    -20.00  21.00   1.00    6.50    --   13.27 -38.00  30.00   41
  3  \w     40.00  86.00   1.00    6.50    --   13.27  38.00  30.00   46
  4  \w      7.00  71.00   1.00    6.50    --   13.27  57.00-150.00   64
  5  \w     -5.00  79.00   1.00    6.50    --   13.27  38.00   0.00   84
  6  \w    -30.00  11.00   1.00    6.50    --   13.27 115.00 -76.00   41
  7  \w    -56.00 -29.00   1.00    6.50    --   13.27 -38.00  30.00   27
  8  \w    -35.00  21.00   1.00    6.50    --   13.27 -38.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0307223000
_diffrn_orient_matrix_UB_12      0.0217917000
_diffrn_orient_matrix_UB_13      -0.0387136000
_diffrn_orient_matrix_UB_21      0.0060710000
_diffrn_orient_matrix_UB_22      0.0350203000
_diffrn_orient_matrix_UB_23      0.0248657000
_diffrn_orient_matrix_UB_31      0.0708569000
_diffrn_orient_matrix_UB_32      0.0064461000
_diffrn_orient_matrix_UB_33      -0.0042821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22528
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.271
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+1.3270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4229
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            md492_mc184.cif
_cod_data_source_block           md492_mc184
_cod_original_cell_volume        2494.73(13)
_cod_database_code               1556594
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.611
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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. Restrained distances
 N1-C2A \\sim N1-C2 \\sim N2-C4A \\sim N2-C4
 with sigma of 0.001
 C2A-C3A \\sim C3-C2 \\sim C4A-C3A \\sim C3-C4
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 N1, N2, C2, H2A, H2B, C3, H3A, H3B, C4, H4A, H4B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.001
 N1, N2, C2A, H2AA, H2AB, C3A, H3AA, H3AB, C4A, H4AA, H4AB
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C3(H3A,H3B), C3A(H3AA,H3AB), C4(H4A,H4B),
 C4A(H4AA,H4AB)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C)
;