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_4070096
_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 H31 Cl2 N2 P S2 Zr'
_chemical_formula_sum            'C32 H31 Cl2 N2 P S2 Zr'
_chemical_formula_weight         700.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.685(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   8.578(5)
_cell_length_b                   19.944(5)
_cell_length_c                   18.983(5)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.5906
_cell_measurement_theta_min      2.3785
_cell_volume                     3244(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28937
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                3826
_reflns_number_total             6164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900612n_si_005.cif
_cod_data_source_block           mf711
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070096