Evidence for the Existence of Group 3 Terminal Methylidene Complexes
Levine, Daniel S.; Tilley, T. Don; Andersen, Richard A.; Organometallics 36 (2017) 80–; doi:10.1021/acs.organomet.6b00394

data_4086839
_publ_section_title
;
 Evidence for the Existence of Group 3 Terminal Methylidene Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              80
_journal_paper_doi               10.1021/acs.organomet.6b00394
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C32 H64 N P2 Y'
_chemical_formula_weight         613.69
_chemical_name_common            (PNP-tBu)YNp2
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                95.262(2)
_cell_angle_beta                 107.167(2)
_cell_angle_gamma                96.588(2)
_cell_formula_units_Z            4
_cell_length_a                   11.2268(4)
_cell_length_b                   18.2514(7)
_cell_length_c                   18.4495(7)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.45
_cell_volume                     3556.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
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_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50816
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.749
_exptl_absorpt_correction_T_max  0.9488
_exptl_absorpt_correction_T_min  0.9321
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         13051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9455
_reflns_number_total             13051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00394_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4086838--4086839.cif.'
_cod_database_code               4086839
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              29813
_shelx_hkl_checksum              87889