Synthesis and structure of early transition metal NHC complexes
Lorber, Christian; Vendier, Laure; Dalton Transactions  (2009) 6972–; doi:10.1039/b905056f

data_7001950
_publ_section_title
;
 Synthesis and structure of early transition metal NHC complexes
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              6972
_journal_paper_doi               10.1039/b905056f
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H25 N2, Cl'
_chemical_formula_sum            'C21 H25 Cl N2'
_chemical_formula_weight         340.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                93.658(9)
_cell_angle_beta                 116.037(11)
_cell_angle_gamma                90.853(9)
_cell_formula_units_Z            8
_cell_length_a                   16.2380(18)
_cell_length_b                   16.3664(16)
_cell_length_c                   16.5630(18)
_cell_measurement_reflns_used    3842
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1467
_cell_measurement_theta_min      2.5755
_cell_measurement_wavelength     0.71073
_cell_volume                     3942.4(8)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.038745927
_diffrn_orient_matrix_UB_12      -0.0218868324
_diffrn_orient_matrix_UB_13      -0.0014262341
_diffrn_orient_matrix_UB_21      0.0286801992
_diffrn_orient_matrix_UB_22      -0.0309640555
_diffrn_orient_matrix_UB_23      0.0243054441
_diffrn_orient_matrix_UB_31      0.0066872478
_diffrn_orient_matrix_UB_32      0.0214687197
_diffrn_orient_matrix_UB_33      0.0411480844
_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  0.0956
_diffrn_reflns_av_unetI/netI     0.3659
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29327
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.95518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         14914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.738
_refine_ls_R_factor_all          0.2065
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                4253
_reflns_number_total             14914
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b905056f.txt
_cod_data_source_block           cl1111
_cod_original_cell_volume        3942.4(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7001950