Synthesis and Characterization of a New Thiophene-Bridged Diamidophosphine [NPN] Donor Set and Its Coordination Chemistry with Zirconium(IV): Unexpected Deprotonation−Lithiation Sequence with a Mesitylaminothiophene Precursor
Ménard, Gabriel; Jong, Howard; Fryzuk, Michael D.; Organometallics 28 (2009) 5253–; doi:10.1021/om900612n

data_4070094
_publ_section_title
;
 Synthesis and Characterization of a New Thiophene-Bridged
 Diamidophosphine [NPN] Donor Set and Its Coordination Chemistry with
 Zirconium(IV): Unexpected Deprotonation&#x2212;Lithiation Sequence with a
 Mesitylaminothiophene Precursor
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              5253
_journal_paper_doi               10.1021/om900612n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C32 H33 N2 P S2'
_chemical_formula_sum            'C32 H33 N2 P S2'
_chemical_formula_weight         540.69
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3490(18)
_cell_length_b                   16.510(3)
_cell_length_c                   25.716(4)
_cell_measurement_reflns_used    8541
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4184
_cell_measurement_theta_min      2.5217
_cell_volume                     5667.6(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'Bruker X8 Apex 2'
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25923
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.97356
_exptl_absorpt_correction_T_min  0.83724
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+2.5684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                4963
_reflns_number_total             6571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900612n_si_003.cif
_cod_data_source_block           mf728
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5667.4(15)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4070094