Multimodal Structure Solution with <sup>19</sup>F NMR Crystallography of Spin Singlet Molybdenum Oxyfluorides.
Ding, Fenghua; Griffith, Kent J.; Koçer, Can P; Saballos, Richard; Wang, Yiran; Zhang, Chi; Nisbet, Matthew L.; Morris, Andrew J.; Rondinelli, James M.; Poeppelmeier, Kenneth R.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c04019

data_4135106
_publ_section_title
;
 Multimodal Structure Solution with <sup>19</sup>F NMR Crystallography of
 Spin Singlet Molybdenum Oxyfluorides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c04019
_journal_year                    2020
_chemical_formula_moiety         '0.5(F72 H8 K32 Mo12 O20 Ti6)'
_chemical_formula_sum            'F36 H4 K16 Mo6 O10 Ti3'
_chemical_formula_weight         2192.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.33680(10)
_cell_length_b                   24.8645(2)
_cell_length_c                   14.71280(10)
_cell_measurement_reflns_used    67101
_cell_measurement_temperature    296.1(3)
_cell_measurement_theta_max      33.9470
_cell_measurement_theta_min      2.7560
_cell_volume                     2311.28(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.1(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_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      8.00  86.00   0.50    5.00    --   13.12  37.00  30.00  156
  2  \w     57.00  86.00   0.50    5.00    --   13.12  37.00 120.00   58
  3  \w      1.00  54.00   0.50    5.00    --   13.12  37.00 120.00  106
  4  \w    -27.00  -1.00   0.50    5.00    --  -13.59 -37.00  30.00   52
  5  \w    -21.00   5.00   0.50    5.00    --   13.12 -99.00   0.00   52
  6  \w     11.00  59.00   0.50    5.00    --   13.12-122.00  12.00   96
  7  \w     21.00  47.00   0.50    5.00    --   13.12 -99.00 120.00   52
  8  \w      7.00  55.00   0.50    5.00    --   13.12-113.00 116.13   96
  9  \w      4.00  55.00   0.50    5.00    --   13.12-113.00  82.01  102
 10  \w     14.00  47.00   0.50    5.00    --   13.12 -99.00   0.00   66
 11  \w     -6.00  47.00   0.50    5.00    --   13.12 -99.00 -60.00  106
 12  \w     34.00  75.00   0.50    5.00    --   13.12-151.00-148.00   82
 13  \w     -2.00  86.00   0.50    5.00    --   13.12  57.00 -60.00  176
 14  \w    -23.00   2.00   0.50    5.00    --   13.12 -99.00 120.00   50
 15  \w    -85.00 -40.00   0.50    5.00    --  -13.59 -37.00  30.00   90
 16  \w      0.00  52.00   0.50    5.00    --   13.12-108.00 -80.68  104
 17  \w    -34.00  -1.00   0.50    5.00    --  -13.59 -19.00-180.00   66
 18  \w    -56.00   1.00   0.50    5.00    --  -13.59 -57.00 -60.00  114
 19  \w    -85.00   8.00   0.50    5.00    --  -13.59 -77.00 120.00  186
 20  \w    -84.00 -58.00   0.50    5.00    --  -13.59 -57.00 -60.00   52
 21  \w    -85.00   8.00   0.50    5.00    --  -13.59 -77.00-180.00  186
 22  \w    -87.00 -62.00   0.50    5.00    --  -13.59 -19.00-180.00   50
 23  \w    -70.00 -41.00   0.50    5.00    --  -13.59 151.00-104.00   58
 24  \w    -59.00 -14.00   0.50    5.00    --  -13.59 122.00  94.00   90
 25  \w    -54.00 -29.00   0.50    5.00    --  -13.59 111.00 127.53   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0854535000
_diffrn_orient_matrix_UB_12      -0.0168812000
_diffrn_orient_matrix_UB_13      -0.0156760000
_diffrn_orient_matrix_UB_21      0.0576750000
_diffrn_orient_matrix_UB_22      -0.0228306000
_diffrn_orient_matrix_UB_23      0.0168134000
_diffrn_orient_matrix_UB_31      -0.0444487000
_diffrn_orient_matrix_UB_32      0.0027999000
_diffrn_orient_matrix_UB_33      0.0425303000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            99039
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.854
_diffrn_reflns_theta_min         2.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.00091(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+2.7432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7959
_reflns_number_total             8617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04019_si_002.cif
_cod_data_source_block           K16[Mo3O4F9]2[TiF6]3_2H2O_(296K)
_cod_database_code               4135106
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H10 N O'
_diffrn_oxdiff_digest_frames
;
0144c5fbba624db0cbb4141c167eeee232022967b5c
;
_diffrn_oxdiff_digest_hkl
;
012ba56ba660fb08042e0460fbad83e3ccb236
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              47497
_shelx_hkl_checksum              34848
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.885