Holmium, thulium and lutetium-octamolybdate [Mo<sub>8</sub>O<sub>28</sub>]<sup>8-</sup> 1D chains: luminescence investigation of europium doped lutetium-octamolybdate.
Kaczmarek, Anna M.; Van Deun, Rik; Van Hecke, Kristof; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8186–8192; doi:10.1039/c9dt00695h

data_7049946
_publ_section_title
;
 Holmium, thulium and lutetium-octamolybdate
 [Mo<sub>8</sub>O<sub>28</sub>]<sup>8-</sup> 1D chains: luminescence
 investigation of europium doped lutetium-octamolybdate.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8186
_journal_page_last               8192
_journal_paper_doi               10.1039/c9dt00695h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'Mo8 O33 Tm, 5(H4N), 7(H2O)'
_chemical_formula_sum            'H34 Mo8 N5 O40 Tm'
_chemical_formula_weight         1680.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-17
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-17 deposited with the CCDC.    2019-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                76.014(2)
_cell_angle_beta                 85.8180(10)
_cell_angle_gamma                84.545(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5985(2)
_cell_length_b                   12.9686(3)
_cell_length_c                   14.4308(3)
_cell_measurement_reflns_used    25064
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.3760
_cell_measurement_theta_min      2.9100
_cell_volume                     1913.40(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     26.00  90.00   1.00    2.00    --   10.17-166.00-176.00   64
  2  \w     -6.00  61.00   1.00    2.00    --   10.17-116.00 -29.00   67
  3  \w    -62.00 -16.00   1.00    2.00    --  -11.03 116.00  58.00   46
  4  \w     -6.00  40.00   1.00    2.00    --  -11.03-116.00 -29.00   46
  5  \w    -66.00  43.00   1.00    2.00    --   10.17 -77.00-120.00  109
  6  \w    -18.00  83.00   1.00    2.00    --   10.17  57.00-180.00  101
  7  \w     35.00  99.00   1.00    2.00    --   10.17 178.00 150.00   64
  8  \w    -36.00  63.00   1.00    2.00    --  -11.03  38.00   0.00   99
  9  \w    -18.00  83.00   1.00    2.00    --   10.17  57.00  60.00  101
 10  \w    -18.00  83.00   1.00    2.00    --   10.17  57.00-120.00  101
 11  \w    -84.00 -37.00   1.00    2.00    --  -11.03 151.00  80.38   47
 12  \w    -84.00 -37.00   1.00    2.00    --  -11.03 151.00 -52.37   47
 13  \w    -66.00 -22.00   1.00    2.00    --  -11.03 123.00 174.16   44
 14  \w    -68.00 -24.00   1.00    2.00    --  -11.03 126.00-105.54   44
 15  \w    -85.00  13.00   1.00    2.00    --  -11.03 -38.00-120.00   98
 16  \w    -20.00  51.00   1.00    2.00    --   10.17 -99.00-180.00   71
 17  \w    -70.00 -39.00   1.00    2.00    --  -11.03 129.00   2.96   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0061992000
_diffrn_orient_matrix_UB_12      -0.0281883000
_diffrn_orient_matrix_UB_13      0.0485637000
_diffrn_orient_matrix_UB_21      -0.0302860000
_diffrn_orient_matrix_UB_22      0.0464934000
_diffrn_orient_matrix_UB_23      0.0121125000
_diffrn_orient_matrix_UB_31      -0.0598013000
_diffrn_orient_matrix_UB_32      -0.0155309000
_diffrn_orient_matrix_UB_33      -0.0082160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            63922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.710
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.946
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.917
_exptl_crystal_description       plate
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.088
_refine_diff_density_max         3.599
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9916
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0519P)^2^+11.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8043
_reflns_number_total             9916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00695h2.cif
_cod_data_source_block           pom80
_cod_depositor_comments
'Adding full bibliography for 7049945--7049947.cif.'
_cod_database_code               7049946
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O41A) = Uanis(O41B)
2. Others
 Sof(O41B)=1-FVAR(1)
 Sof(O41A)=FVAR(1)
;
_shelx_res_checksum              53255
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.649