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_7049947
_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         'Lu Mo8 O33, 5(H4N), 7(H2O)'
_chemical_formula_sum            'H34 Lu Mo8 N5 O40'
_chemical_formula_weight         1687.93
_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                76.258(2)
_cell_angle_beta                 84.894(3)
_cell_angle_gamma                84.370(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5090(4)
_cell_length_b                   12.9322(3)
_cell_length_c                   14.3629(4)
_cell_measurement_reflns_used    12101
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.6650
_cell_measurement_theta_min      2.9120
_cell_volume                     1882.60(10)
_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_environment      N~2~
_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 0.884
_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     13.00  79.00   1.00   15.00    --   10.33-145.00  15.00   66
  2  \w      3.00  67.00   1.00   15.00    --   10.33-126.00-176.00   64
  3  \w    -14.00  85.00   1.00   15.00    --   10.33  38.00   0.00   99
  4  \w    -22.00  86.00   1.00   15.00    --   10.33  77.00 -90.00  108
  5  \w    -66.00  43.00   1.00   15.00    --   10.33 -77.00  60.00  109
  6  \w    -78.00 -33.00   1.00   15.00    --  -11.19 142.00 -17.55   45
  7  \w    -85.00  13.00   1.00   15.00    --  -11.19 -38.00-150.00   98
  8  \w    -20.00  30.00   1.00   15.00    --  -11.19 -99.00 150.00   50
  9  \w    -31.00  90.00   1.00   15.00    --   10.33  19.00 150.00  121
 10  \w    -87.00 -62.00   1.00   15.00    --  -11.19 154.00-169.32   25
;
_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      -0.0409012000
_diffrn_orient_matrix_UB_12      0.0110144000
_diffrn_orient_matrix_UB_13      -0.0384634000
_diffrn_orient_matrix_UB_21      0.0533158000
_diffrn_orient_matrix_UB_22      0.0131130000
_diffrn_orient_matrix_UB_23      -0.0332326000
_diffrn_orient_matrix_UB_31      0.0102778000
_diffrn_orient_matrix_UB_32      -0.0539925000
_diffrn_orient_matrix_UB_33      -0.0035773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41947
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.792
_diffrn_reflns_theta_min         2.426
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.293
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.822
_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    2.978
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1593
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.661
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0386P)^2^+5.8696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6977
_reflns_number_total             9509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00695h2.cif
_cod_data_source_block           pom82
_cod_depositor_comments
'Adding full bibliography for 7049945--7049947.cif.'
_cod_database_code               7049947
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.86
_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)
Uanis(O42A) = Uanis(O42B)
Uanis(O45A) = Uanis(O45B)
2. Others
 Sof(O41B)=1-FVAR(1)
 Sof(O41A)=FVAR(1)
 Sof(O42B)=Sof(O42A)=FVAR(2)
 Sof(O45B)=1-FVAR(3)
 Sof(O45A)=FVAR(3)
;
_shelx_res_checksum              29035
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.791