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_7017542
_publ_section_related_literature
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?
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_publ_section_title
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 Novel heterometal-organic complexes as first single source precursors for
 up-converting NaY(Ln)F(4) (Ln = Yb, Er, Tm) nanomaterials.
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_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_formula_moiety         'C22 H16 F21 O16 Y2, C16 H36 Na O8'
_chemical_formula_sum            'C38 H52 F21 Na O24 Y2'
_chemical_formula_weight         1492.61
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                   29.260(4)
_cell_length_b                   11.8630(10)
_cell_length_c                   18.725(2)
_cell_measurement_reflns_used    3538
_cell_measurement_temperature    180
_cell_measurement_theta_max      29.3474
_cell_measurement_theta_min      3.0993
_cell_volume                     6499.7(13)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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      180
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.095
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7725
_diffrn_reflns_theta_full        25.029
_diffrn_reflns_theta_max         29.445
_diffrn_reflns_theta_min         3.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.43
_refine_diff_density_min         -2.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.2072
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.0004611
_refine_ls_shift/su_mean         0.0000377
_refine_ls_structure_factor_coef Fsqd
_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:
965. 0.124E+04 378.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1857
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1857
_reflns_limit_h_max              39
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                2334
_reflns_number_total             7725
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.2072
_oxford_refine_ls_scale          1.622(11)
_oxford_reflns_number_all        7725
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr147 in P c c a'
_cod_data_source_file            c1dt11070e.txt
_cod_data_source_block           complex2
_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 c c a '
_cod_database_code               7017542
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'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)
RIDE C ( 11,X'S) H ( 112,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,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)
RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S)
RIDE C ( 47,X'S) H ( 472,X'S) H ( 471,X'S)
RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S)
RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S)
RIDE C ( 52,X'S) H ( 522,X'S) H ( 521,X'S) H ( 523,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)
DISTANCE 1.250000 , 0.010000 = F(7) TO C(4)
DISTANCE 1.250000 , 0.010000 = F(8) TO C(4)
DISTANCE 1.250000 , 0.010000 = F(9) TO C(4)
DISTANCE 1.250000 , 0.010000 = F(5) TO C(2)
DISTANCE 1.250000 , 0.010000 = F(4) TO C(2)
DISTANCE 1.250000 , 0.010000 = F(13) TO C(8)
DISTANCE 1.250000 , 0.010000 = F(14) TO C(8)
DISTANCE 1.250000 , 0.010000 = F(15) TO C(8)
DISTANCE 1.250000 , 0.010000 = F(16) TO C(8)
DISTANCE 1.250000 , 0.010000 = F(17) TO C(8)
DISTANCE 1.250000 , 0.010000 = F(18) TO C(8)
U(IJ)'S 0.0, 0.0050000 = F(7) TO F(8)
U(IJ)'S 0.0, 0.0050000 = F(8) TO F(9)
U(IJ)'S 0.0, 0.0050000 = F(13) TO F(14)
U(IJ)'S 0.0, 0.005000 = F(14) TO F(15)
U(IJ)'S 0.0, 0.005000 = F(15) TO F(16)
U(IJ)'S 0.0, 0.005000 = F(16) TO F(17)
U(IJ)'S 0.0, 0.005000 = F(17) TO F(18)
U(IJ)'S 0.0, 0.005000 = F(1) TO F(2)
U(IJ)'S 0.0, 0.005000 = F(2) TO F(3)
U(IJ)'S 0.0, 0.005000 = F(3) TO F(4)
U(IJ)'S 0.0, 0.005000 = F(4) TO F(5)
U(IJ)'S 0.0, 0.005000 = F(5) TO F(6)
U(IJ)'S 0.0, 0.010000 = C(7) TO C(8)
U(IJ)'S 0.0, 0.010000 = C(1) TO C(2)
U(IJ)'S 0.0, 0.010000 = F(7) TO C(4)
U(IJ)'S 0.0, 0.010000 = F(8) TO C(4)
U(IJ)'S 0.0, 0.010000 = F(9) TO C(4)
U(IJ)'S 0.0, 0.010000 = C(3) TO C(4)
U(IJ)'S 0.0, 0.010000 = C(5) TO C(6)
U(IJ)'S 0.0, 0.010000 = F(10) TO C(6)
U(IJ)'S 0.0, 0.010000 = F(11) TO C(6)
U(IJ)'S 0.0, 0.010000 = F(12) TO C(6)
END
;