Compelling mechanistic data and identification of the active species in tungsten-catalyzed alkyne polymerizations: conversion of a trianionic pincer into a new tetraanionic pincer-type ligand
McGowan, Kevin P.; O'Reilly, Matthew E.; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Chemical Science 4 (2013) 1145–; doi:10.1039/c2sc21750c

data_1514561
_publ_section_title
;
 Compelling mechanistic data and identification of the active species in
 tungsten-catalyzed alkyne polymerizations: conversion of a trianionic
 pincer into a new tetraanionic pincer-type ligand
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              1145
_journal_paper_doi               10.1039/c2sc21750c
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C48 H50 O2 W1, 0.5(C4 H10 O1)'
_chemical_formula_sum            'C50 H55 O2.5 W'
_chemical_formula_weight         879.79
_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
_audit_update_record
;
2012-08-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.047(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6683(5)
_cell_length_b                   40.736(2)
_cell_length_c                   21.0306(13)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.46
_cell_volume                     8220.3(8)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73336
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         18795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                12987
_reflns_number_total             18795
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2sc21750c.txt
_cod_data_source_block           mcg9
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_original_formula_sum        'C50 H55 O2.50 W'
_cod_database_code               1514561