Alkaline Earth Metal‒Carbene Complexes with the Versatile Tridentate 2,6-Bis(3-mesitylimidazol-2-ylidene)pyridine Ligand
Koch, Alexander; Krieck, Sven; Görls, Helmar; Westerhausen, Matthias; Organometallics 36 (2017) 994–; doi:10.1021/acs.organomet.6b00914

data_4087077
_publ_section_title
;
 Alkaline Earth Metal--Carbene Complexes with the Versatile Tridentate
 2,6-Bis(3-mesitylimidazol-2-ylidene)pyridine Ligand
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              994
_journal_paper_doi               10.1021/acs.organomet.6b00914
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         '2(C62 H66 Ca N10 O), 7(C4 H8 O), 4(I)'
_chemical_formula_sum            'C76 H94 Ca I2 N10 O4.5'
_chemical_formula_weight         1513.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 110.368(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3225(6)
_cell_length_b                   15.7849(5)
_cell_length_c                   24.0166(7)
_cell_measurement_reflns_used    77598
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.68
_cell_volume                     7222.6(4)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            77598
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            light_yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.082
_refine_diff_density_max         2.072
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         15308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+27.0858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                12828
_reflns_number_total             15308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00914_si_001.cif
_cod_data_source_block           FO5921
_cod_depositor_comments
'Adding full bibliography for 4087076--4087082.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C76 H94 Ca I2 N10 O4.50'
_cod_database_code               4087077