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_7049945
_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         'Ho Mo8 O33 H12, 5(H4N), 8(H2O)'
_chemical_formula_sum            'H48 Ho Mo8 N5 O41'
_chemical_formula_weight         1694.79
_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                76.253(3)
_cell_angle_beta                 84.980(3)
_cell_angle_gamma                84.373(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5227(4)
_cell_length_b                   12.9748(5)
_cell_length_c                   14.3537(4)
_cell_measurement_reflns_used    12050
_cell_measurement_temperature    100.1(2)
_cell_measurement_theta_max      75.2290
_cell_measurement_theta_min      3.1500
_cell_volume                     1890.22(12)
_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      100.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_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   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00 -90.00   99
  2  \w    -66.00  33.00   1.00    2.00    --  -41.68  38.00  90.00   99
  3  \w     23.00  98.00   1.00    2.00    --   41.68-125.00 -60.00   75
  4  \w      1.00  83.00   1.00    2.00    --   41.68 -99.00  60.00   82
  5  \w      9.00 118.00   1.00    2.00    --   41.68  77.00-180.00  109
  6  \w     26.00 110.00   1.00    9.00    --  109.13 -94.00  60.00   84
  7  \w     36.00 106.00   1.00    9.00    --  109.13-125.00-180.00   70
  8  \w     36.00 135.00   1.00    9.00    --  109.13 -45.00 -30.00   99
  9  \w     36.00 117.00   1.00    9.00    --  109.13-125.00  30.00   81
 10  \w     36.00 106.00   1.00    9.00    --  109.13-125.00 -60.00   70
 11  \w     80.00 178.00   1.00    9.00    --  109.13  61.00 120.00   98
 12  \w     83.00 178.00   1.00    9.00    --  109.13  45.00-120.00   95
 13  \w     81.00 178.00   1.00    9.00    --  109.13  30.00-150.00   97
 14  \w    101.00 178.00   1.00    9.00    --  109.13 104.00 -42.00   77
 15  \w     37.00 138.00   1.00    9.00    --  109.13 -61.00 120.00  101
 16  \w     94.00 178.00   1.00    9.00    --  109.13 125.00  60.00   84
 17  \w   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00  90.00   99
 18  \w   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00  30.00  101
 19  \w      9.00 118.00   1.00    2.00    --   41.68  77.00 -90.00  109
 20  \w    -33.00  66.00   1.00    2.00    --   41.68 -38.00 150.00   99
 21  \w      9.00 118.00   1.00    2.00    --   41.68  77.00  60.00  109
 22  \w     81.00 178.00   1.00    9.00    --  109.13  30.00 -60.00   97
 23  \w     80.00 178.00   1.00    9.00    --  109.13  61.00   0.00   98
 24  \w     56.00 178.00   1.00    9.00    --  109.13  15.00  30.00  122
 25  \w     80.00 178.00   1.00    9.00    --  109.13  61.00  90.00   98
 26  \w     80.00 178.00   1.00    9.00    --  109.13  61.00  30.00   98
 27  \w     80.00 178.00   1.00    9.00    --  109.13  61.00 150.00   98
 28  \w     80.00 178.00   1.00    9.00    --  109.13  61.00 -60.00   98
 29  \w     77.00 178.00   1.00    9.00    --  109.13  77.00-180.00  101
 30  \w     80.00 178.00   1.00    9.00    --  109.13  61.00 -30.00   98
 31  \w     80.00 178.00   1.00    9.00    --  109.13  61.00  60.00   98
 32  \w      9.00 104.00   1.00    2.00    --   41.68  77.00 -30.00   95
 33  \w      1.00  83.00   1.00    2.00    --   41.68 -99.00 -30.00   82
;
_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      -0.1416117000
_diffrn_orient_matrix_UB_12      -0.0232857000
_diffrn_orient_matrix_UB_13      0.0058090000
_diffrn_orient_matrix_UB_21      0.0088760000
_diffrn_orient_matrix_UB_22      -0.0580539000
_diffrn_orient_matrix_UB_23      0.1064088000
_diffrn_orient_matrix_UB_31      -0.0400644000
_diffrn_orient_matrix_UB_32      0.1054756000
_diffrn_orient_matrix_UB_33      0.0301041000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35880
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.273
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_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       needle
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.042
_refine_diff_density_max         3.234
_refine_diff_density_min         -2.429
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7644
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0616P)^2^+110.4941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6472
_reflns_number_total             7644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00695h2.cif
_cod_data_source_block           hopom_redo2
_cod_depositor_comments
'Adding full bibliography for 7049945--7049947.cif.'
_cod_database_code               7049945
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
;
_shelx_res_checksum              75178
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 5.270
_oxdiff_exptl_absorpt_empirical_full_min 0.478