Thermally stable rare earth dialkyl complexes supported by a novel bis(phosphinimine)pyrrole ligand.
Johnson, Kevin R. D.; Hannon, Matt A.; Ritch, Jamie S.; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 7873–7875; doi:10.1039/c2dt12485h

data_7019242
_publ_section_title
;
 Thermally stable rare earth dialkyl complexes supported by a novel
 bis(phosphinimine)pyrrole ligand.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7873
_journal_page_last               7875
_journal_paper_doi               10.1039/c2dt12485h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C46 H45 N3 P2'
_chemical_formula_weight         701.79
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.5870(10)
_cell_angle_beta                 103.5210(10)
_cell_angle_gamma                108.7700(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9263(2)
_cell_length_b                   14.5326(2)
_cell_length_c                   14.8331(3)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.53
_cell_volume                     2223.03(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36845
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski & Minor, 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
'A heavily disordered molecule of toluene was present in
the unit cell, for which no suitable model could be found.
The electron density associated with this fragment was
removed using SQUEEZE (PLATON), leaving a void of ca.
386 A^3.'
;
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         10171
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+2.5948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1821
_reflns_number_gt                7370
_reflns_number_total             10171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12485h.txt
_cod_data_source_block           ph11018a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7019242