Synthesis, structures and reactivity of 2-phosphorylmethyl-1H-pyrrolato complexes of titanium, yttrium and zinc
Broomfield, Lewis M.; Wright, Joseph A.; Bochmann, Manfred; Dalton Transactions  (2009) 8269–8279; doi:10.1039/b908394d

data_7002383
_publ_section_title
;
 Synthesis, structures and reactivity of 2-phosphorylmethyl-1H-pyrrolato
 complexes of titanium, yttrium and zinc
;
_journal_coden_ASTM              DTARAF
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8269
_journal_page_last               8279
_journal_paper_doi               10.1039/b908394d
_journal_year                    2009
_chemical_formula_moiety         'C38 H66 N4 O2 P2 Ti'
_chemical_formula_structural     '[Pyr-P(O)Cy2]2Ti(NMe2)2'
_chemical_formula_sum            'C38 H66 N4 O2 P2 Ti'
_chemical_formula_weight         720.79
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.173(3)
_cell_angle_beta                 88.666(2)
_cell_angle_gamma                89.788(3)
_cell_formula_units_Z            4
_cell_length_a                   10.7254(5)
_cell_length_b                   19.2509(7)
_cell_length_c                   19.6142(8)
_cell_measurement_reflns_used    128503
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4000.8(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44782
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.9837
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/2; Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.670
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1244
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1658P)^2^+36.7696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3093
_refine_ls_wR_factor_ref         0.3343
_reflns_number_gt                8151
_reflns_number_total             10375
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908394D.txt
_cod_data_source_block           5d
_cod_database_code               7002383