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_7002385
_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         'C51 H45 N3 O3 P3 Y, C7 H8'
_chemical_formula_structural     '[Pyr-P(O)Ph2]3Y.PhMe'
_chemical_formula_sum            'C58 H53 N3 O3 P3 Y'
_chemical_formula_weight         1021.85
_chemical_name_common            'Compound 8a'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 127.768(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.899(3)
_cell_length_b                   18.890(3)
_cell_length_c                   22.165(3)
_cell_measurement_reflns_used    1368
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4279
_cell_volume                     4931.3(16)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.005
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3797
_diffrn_reflns_av_sigmaI/netI    0.4040
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40276
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  0.9498
_exptl_absorpt_correction_T_min  0.7845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     622
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.2801
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                1968
_reflns_number_total             6410
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b908394D.txt
_cod_data_source_block           8a
_cod_original_cell_volume        4931.2(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002385