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_1556595
_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         'C38 H47 Ga N2 O'
_chemical_formula_sum            'C38 H47 Ga N2 O'
_chemical_formula_weight         617.49
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 100.916(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5312(3)
_cell_length_b                   18.7807(5)
_cell_length_c                   19.0639(5)
_cell_measurement_reflns_used    14264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4370
_cell_measurement_theta_min      3.9090
_cell_volume                     4053.85(19)
_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    -12.00  83.00   1.00    8.00    --   14.72  38.00   0.00   95
  2  \w     18.00  91.00   1.00    8.00    --   14.72  38.00 150.00   73
  3  \w    -18.00  75.00   1.00    8.00    --   14.72  77.00  30.00   93
  4  \w    -15.00  89.00   1.00    8.00    --   14.72  57.00-120.00  104
  5  \w    -54.00  44.00   1.00    8.00    --   14.72 -77.00-120.00   98
  6  \w    -93.00 -16.00   1.00    8.00    --  -14.40 156.00 -42.93   77
  7  \w    -93.00 -19.00   1.00    8.00    --  -14.40 156.00  57.47   74
  8  \w    -93.00 -16.00   1.00    8.00    --  -14.40 156.00-124.88   77
;
_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      0.0270479000
_diffrn_orient_matrix_UB_12      0.0176951000
_diffrn_orient_matrix_UB_13      0.0317632000
_diffrn_orient_matrix_UB_21      0.0557036000
_diffrn_orient_matrix_UB_22      -0.0136467000
_diffrn_orient_matrix_UB_23      -0.0040199000
_diffrn_orient_matrix_UB_31      0.0092326000
_diffrn_orient_matrix_UB_32      0.0304791000
_diffrn_orient_matrix_UB_33      -0.0202549000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66718
_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    1.012
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.99
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0418P)^2^+0.9608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6377
_reflns_number_total             8392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            md493_MC188_sq.cif
_cod_data_source_block           md493_mc188_sq
_cod_original_cell_volume        4053.87(19)
_cod_database_code               1556595
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
2.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), C26(H26A,H26B,H26C)
;