New Alkylidyne Complexes Featuring a Flexible Trianionic ONO3‒ Pincer-Type Ligand: Inorganic Enamine Effect versus Sterics in Electrophilic Additions
VenkatRamani, Sudarsan; Huff, Nicholas B.; Jan, Muhammad Tariq; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Organometallics 34 (2015) 2841–; doi:10.1021/acs.organomet.5b00155

data_4087478
_publ_section_title
;
 New Alkylidyne Complexes Featuring a Flexible Trianionic ONO3--
 Pincer-Type Ligand: Inorganic Enamine Effect versus Sterics in
 Electrophilic Additions
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2841
_journal_paper_doi               10.1021/acs.organomet.5b00155
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H46 N1 O3 W1, C19 H18 P1, 1.5(C6 H6)'
_chemical_formula_sum            'C59 H73 N O3 P W'
_chemical_formula_weight         1059.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-03-24 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.692(3)
_cell_length_b                   14.3559(11)
_cell_length_c                   20.7640(15)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     10639.3(14)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1736
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            170485
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.529
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.8439
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plates
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.080
_refine_diff_density_min         -2.275
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         12232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6292
_reflns_number_total             12232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00155_si_004.cif
_cod_data_source_block           sud9
_cod_original_cell_volume        10639.4(14)
_cod_database_code               4087478
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.922
_shelxl_version_number           2013-3
_shelx_res_checksum              9349
_shelx_hkl_checksum              3764