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_7039742
_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 Er4 N24 O32), 3(C F3 O3 S)'
_chemical_formula_sum            'C33 H28 Er F9 N6 O17 S3'
_chemical_formula_weight         1215.05
_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                   16.7834(5)
_cell_length_b                   13.8374(4)
_cell_length_c                   20.1138(4)
_cell_measurement_reflns_used    2998
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      28.4840
_cell_measurement_theta_min      3.7550
_cell_volume                     4671.2(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)'
_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 0.869
_diffrn_measurement_details
;
  1 omega    9.00   51.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0343  -99.0000  -30.0000 42

  2 omega  -85.00   27.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7374    0.0000   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      0.0309539000
_diffrn_orient_matrix_UB_12      -0.0184667000
_diffrn_orient_matrix_UB_13      0.0203614000
_diffrn_orient_matrix_UB_21      0.0021291000
_diffrn_orient_matrix_UB_22      -0.0418892000
_diffrn_orient_matrix_UB_23      -0.0202296000
_diffrn_orient_matrix_UB_31      0.0286569000
_diffrn_orient_matrix_UB_32      0.0230995000
_diffrn_orient_matrix_UB_33      -0.0205047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13592
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.175
_diffrn_reflns_theta_min         3.488
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85382
_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            Orange
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.135
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         13592
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+8.2449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9495
_reflns_number_total             13592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01828a2.cif
_cod_data_source_block           bc5
_cod_depositor_comments
'Adding full bibliography for 7039742--7039746.cif.'
_cod_database_code               7039742
_chemical_oxdiff_formula         'Er C10 N2 H10 O11 F9 S3'
_reflns_odcompleteness_completeness 99.57
_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. 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}
3. 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)
4.a Rotating group:
 O4W(H4WA,H4WB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C5(H5), C4(H4), C15(H15), C14(H14), C11(H11), C12(H12),
 C6(H6), C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              66814
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'