Fine-Tunable 3,4-Dihydroquinazol-2-ylidene Carbenes: Synthesis, Rhodium(I) Complexes, and Reactivity
Zhang, Jun; Qin, Xinke; Fu, Jun; Wang, Xiao; Su, Xiaolong; Hu, Fangle; Jiao, Jiajun; Shi, Min; Organometallics 31 (2012) 8275–; doi:10.1021/om300887y

data_4083260
_publ_section_title
;
 Fine-Tunable 3,4-Dihydroquinazol-2-ylidene Carbenes: Synthesis,
 Rhodium(I) Complexes, and Reactivity
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8275
_journal_paper_doi               10.1021/om300887y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C25 H36 Cl N2 Rh'
_chemical_formula_weight         502.92
_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                90.00
_cell_angle_beta                 110.777(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.471(4)
_cell_length_b                   14.344(5)
_cell_length_c                   15.534(6)
_cell_measurement_reflns_used    896
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.952
_cell_measurement_theta_min      3.428
_cell_volume                     2389.7(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10564
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        3.56
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.7576
_exptl_absorpt_correction_T_min  0.6240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                3719
_reflns_number_total             4666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300887y_si_001.cif
_cod_data_source_block           a20326a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4083260