Novel heterometal-organic complexes as first single source precursors for up-converting NaY(Ln)F(4) (Ln = Yb, Er, Tm) nanomaterials.
Mishra, Shashank; Ledoux, Gilles; Jeanneau, Erwann; Daniele, Stéphane; Joubert, Marie-France; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1490–1502; doi:10.1039/c1dt11070e

data_7017543
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Novel heterometal-organic complexes as first single source precursors for
 up-converting NaY(Ln)F(4) (Ln = Yb, Er, Tm) nanomaterials.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1490
_journal_page_last               1502
_journal_paper_doi               10.1039/c1dt11070e
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H54 F30 Na4 O31 Y2'
_chemical_formula_sum            'C44 H54 F30 Na4 O31 Y2'
_chemical_formula_weight         1918.60
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n 2a'
_symmetry_space_group_name_H-M   'P 21 c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-09-06
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8642(3)
_cell_length_b                   19.6674(4)
_cell_length_c                   21.2130(4)
_cell_measurement_reflns_used    8907
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     7453.0(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16664
_diffrn_reflns_theta_full        25.078
_diffrn_reflns_theta_max         27.864
_diffrn_reflns_theta_min         1.412
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  0.8710
_exptl_absorpt_correction_T_min  0.8271
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 J. de Meulenaar and H. Tompa, Acta Crystallogr., Sect A 1965, 19, 1014-1018.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.32
_refine_diff_density_min         -1.02
_refine_ls_abs_structure_details 'Flack (1983), 7093 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.472(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9499
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         16167
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.0013038
_refine_ls_shift/su_mean         0.0000584
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +13.27P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1802
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1802
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                10306
_reflns_number_total             16181
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.13
_oxford_diffrn_Wilson_scale      289.62
_oxford_refine_ls_r_factor_ref   0.1139
_oxford_refine_ls_scale          0.14275(7)
_oxford_reflns_number_all        16167
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'import in P 21 c n'
_cod_data_source_file            c1dt11070e.txt
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 c n '
_cod_database_code               7017543
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT ENANTIO
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) H ( 103,X'S)
RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S)
RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S)
RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S)
RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S)
RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S)
RIDE C ( 38,X'S) H ( 381,X'S) H ( 382,X'S)
RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S)
RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S) H ( 403,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = C(1) TO C(10)
U(IJ)'S 0.0, 0.010000 = C(2) TO C(9)
U(IJ)'S 0.0, 0.010000 = C(3) TO C(8)
U(IJ)'S 0.0, 0.010000 = O(1) TO O(5)
U(IJ)'S 0.0, 0.010000 = C(41) TO C(44)
U(IJ)'S 0.0, 0.010000 = C(42) TO C(43)
DISTANCE 1.550000 , 0.020000 = C(43) TO C(44)
;