Syntheses, structures and multinuclear NMR (45Sc, 89Y, 31P) studies of Ph3PO, Ph2MePO and Me3PO complexes of scandium and yttrium nitrates
Deakin, Lucy; Levason, William; Popham, Michael C.; Reid, Gillian; Webster, Michael; Journal of the Chemical Society, Dalton Transactions  (2000) 2439–; doi:10.1039/b001669l

data_7009528
_publ_section_title
;
 Syntheses, structures and multinuclear NMR (45Sc, 89Y, 31P) studies of
 Ph3PO, Ph2MePO and Me3PO complexes of scandium and yttrium nitrates
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2439
_journal_paper_doi               10.1039/b001669l
_journal_year                    2000
_chemical_formula_moiety         'C52 H52 N2 O10 P4 Sc, N O3, 1.3(C H2 Cl2)'
_chemical_formula_sum            'C53.3 H54.6 Cl2.6 N3 O13 P4 Sc'
_chemical_formula_weight         1206.21
_chemical_name_systematic
; 
 bis(nitrato-O,O')tetrakis(diphenylmethylphosphineoxide)scandium(III) 
 nitrate dichloromethane solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 98.40(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.712(5)
_cell_length_b                   23.412(4)
_cell_length_c                   18.650(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5923(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku AFC7S diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed fine-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.1679
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10865
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2498
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         10398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.2183
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2460
_refine_ls_wR_factor_ref         0.3322
_reflns_number_gt                4535
_reflns_number_total             10398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001669l.txt
_cod_data_source_block           Elev99_6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21 /n'
_cod_original_formula_sum        'C53.30 H54.60 Cl2.60 N3 O13 P4 Sc'
_cod_database_code               7009528