1,4- to 1,5-Homologation of Alkene-Carbene and Alkyne-Carbene Complexes of Chromium and Tungsten: The Clue to Reactivity
Rudler, Henri; Parlier, Andrée; del Pilar Peregrina, Maria; Vaissermann, Jacqueline; Organometallics 24 (2005) 1–3; doi:10.1021/om0491286

data_4085611
_publ_section_title
;
 1,4- to 1,5-Homologation of Alkene-Carbene and Alkyne-Carbene Complexes
 of Chromium and Tungsten: The Clue to Reactivity
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              1
_journal_page_last               3
_journal_paper_doi               10.1021/om0491286
_journal_volume                  24
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C19 H16 O3'
_chemical_formula_sum            'C19 H16 O3'
_chemical_formula_weight         292.33
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.38(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.271(3)
_cell_length_b                   19.028(6)
_cell_length_c                   9.7530(12)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    295
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     1499.2(8)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.08
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8766
_diffrn_reflns_theta_full        19.250
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.138
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.00
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1113
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1404
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000547
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.463 0.440 0.238 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1506
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0739
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1404
_reflns_number_total             2653
_reflns_threshold_expression     I>1.50u(I)
_cod_data_source_file            Organometallics_2005_1.cif
_cod_data_source_block           C19H16O3
_cod_original_cell_volume        1499.2(7)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4085611
_refine_ls_r_factor_ref          0.0721
_reflns_number_all               2651