Zwitterionic bis(phenolate)amine lanthanide complexes for the ring-opening polymerisation of cyclic esters
Dyer, Hellen E.; Huijser, Saskia; Schwarz, Andrew D.; Wang, Chao; Duchateau, Robbert; Mountford, Philip; Dalton Transactions  (2008) 32–; doi:10.1039/b714583g

data_7003232
_publ_section_title
;
 Zwitterionic bis(phenolate)amine lanthanide complexes for the
 ring-opening polymerisation of cyclic esters
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              32
_journal_paper_doi               10.1039/b714583g
_journal_year                    2008
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C68 H109 N4 O4 Sm1 '
_chemical_formula_sum            'C68 H109 N4 O4 Sm'
_chemical_formula_weight         1197.04
_chemical_name_common            Sm(O2NNMe2)(HO2NNMe2)
_chemical_name_systematic
;
Sm(O2NNMe2)(HO2NNMe2)
;
_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
_cell_angle_alpha                71.0528(5)
_cell_angle_beta                 78.8309(5)
_cell_angle_gamma                87.3893(7)
_cell_formula_units_Z            2
_cell_length_a                   13.4576(2)
_cell_length_b                   16.7022(2)
_cell_length_c                   18.5409(2)
_cell_measurement_reflns_used    55403
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     3866.33(9)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            55403
_diffrn_reflns_theta_full        27.483
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         5.108
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_thermal_history
;
The material was crystallised at 223K. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction
analysis.
;
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         12786
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.042493
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994,
Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and
x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.291 0.0703 0.0986
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0553
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0370
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12786
_reflns_number_total             17496
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b714583g.txt
_cod_data_source_block           Compound_3NMe2
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C68 H109 N4 O4 Sm1 '
_cod_database_code               7003232