Structure and efficient luminescence upconversion of Ln(iii) aromatic N-oxide coordination polymers.
Chong, Bowie S. K.; Moore, Evan G.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12200–12205; doi:10.1039/c6dt01828a

data_7039744
_publ_section_title
;
 Structure and efficient luminescence upconversion of Ln(iii) aromatic
 N-oxide coordination polymers.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12200
_journal_page_last               12205
_journal_paper_doi               10.1039/c6dt01828a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'0.25(C120 H112 Er0.8 N24 O32 Yb3.2), 3(C F3 O3 S)'
_chemical_formula_sum            'C33 H28 Er0.2 F9 N6 O17 S3 Yb0.8'
_chemical_formula_weight         1219.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-09 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7519(3)
_cell_length_b                   13.8277(5)
_cell_length_c                   20.0855(5)
_cell_measurement_reflns_used    3648
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      28.5100
_cell_measurement_theta_min      3.7720
_cell_volume                     4652.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      190.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0696
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega  -77.00  -49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5812 -178.0000  -30.0000 28

  2 omega  -74.00  -38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5812 -178.0000  150.0000 36

  3 omega  -58.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5812   19.0000  -30.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0294228000
_diffrn_orient_matrix_UB_12      0.0327093000
_diffrn_orient_matrix_UB_13      -0.0117867000
_diffrn_orient_matrix_UB_21      0.0287562000
_diffrn_orient_matrix_UB_22      0.0219594000
_diffrn_orient_matrix_UB_23      -0.0210307000
_diffrn_orient_matrix_UB_31      -0.0100398000
_diffrn_orient_matrix_UB_32      -0.0328621000
_diffrn_orient_matrix_UB_33      -0.0257886000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15503
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.170
_diffrn_reflns_theta_min         3.493
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       block
_exptl_crystal_F_000             2410
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.710
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         15503
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+5.1955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10758
_reflns_number_total             15503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01828a2.cif
_cod_data_source_block           bc8_f
_cod_depositor_comments
'Adding full bibliography for 7039742--7039746.cif.'
_cod_original_formula_sum        'C33 H28 Er0.20 F9 N6 O17 S3 Yb0.80'
_cod_database_code               7039744
_chemical_oxdiff_formula         'Er Yb C10 N2 H10 O11 F9 S3'
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Yb1, Er1}
3. Uiso/Uaniso restraints and constraints
Uanis(Yb1) = Uanis(Er1)
4. Same fragment restrains
{S1, O1S, O2S, O3S, C1S, F1, F2, F3} sigma for 1-2: 0.05, 1-3: 0.05
as
{S2, O4S, O5S, O6S, C2S, F4, F5, F6}
{S1, O1S, O2S, O3S, C1S, F1, F2, F3} sigma for 1-2: 0.05, 1-3: 0.05
as
{S2B, O4SB, O5SB, O6SB, C2SB, F4B, F5B, F6B}
5. Others
 Sof(S2B)=Sof(O4SB)=Sof(O5SB)=Sof(O6SB)=Sof(C2SB)=Sof(F4B)=Sof(F5B)=Sof(F6B)=
 0.5*(1-FVAR(2))
 Sof(S2)=Sof(O4S)=Sof(O5S)=Sof(O6S)=Sof(C2S)=Sof(F4)=Sof(F5)=Sof(F6)=0.5*FVAR(2)
 Fixed Sof: Yb1(0.4) Er1(0.1)
6.a Rotating group:
 O4W(H4WA,H4WB)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15)
;
_shelx_res_checksum              83431
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'