A new ONO(3-) trianionic pincer ligand with intermediate flexibility and its tungsten alkylidene and alkylidyne complexes.
VenkatRamani, Sudarsan; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18475–18486; doi:10.1039/c5dt02911b

data_7036384
_publ_section_title
;
 A new ONO(3-) trianionic pincer ligand with intermediate flexibility and
 its tungsten alkylidene and alkylidyne complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18475
_journal_page_last               18486
_journal_paper_doi               10.1039/c5dt02911b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H60 N1 O3 W1, C19 H18 P1, 0.5(C5 H12)'
_chemical_formula_sum            'C59.5 H84 N O3 P W'
_chemical_formula_weight         1076.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-07-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3665(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1363(3)
_cell_length_b                   17.4732(4)
_cell_length_c                   22.8371(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     5565.7(2)
_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 CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0624
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            126389
_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         27.500
_diffrn_reflns_theta_min         1.587
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.146
_exptl_absorpt_correction_T_max  0.9015
_exptl_absorpt_correction_T_min  0.7239
_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    1.284
_exptl_crystal_description       plates
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         12808
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10167
_reflns_number_total             12808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02911b2.cif
_cod_data_source_block           sud13
_cod_depositor_comments
'Adding full bibliography for 7036383--7036384.cif.'
_cod_original_formula_sum        'C59.50 H84 N O3 P W'
_cod_database_code               7036384
_shelx_estimated_absorpt_t_min   0.598
_shelx_estimated_absorpt_t_max   0.875
_shelxl_version_number           2014/6
_shelx_res_checksum              50284