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_4135105
_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             2020-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6464(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.31509(9)
_cell_length_b                   24.7024(3)
_cell_length_c                   14.59723(18)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.22
_cell_measurement_theta_min      2.84
_cell_volume                     2269.65(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      100.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54140
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.781
_diffrn_reflns_theta_min         2.163
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.750
_exptl_absorpt_correction_T_max  0.7401
_exptl_absorpt_correction_T_min  0.6037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0841 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.8030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00061(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   1.062
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8285
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0173
_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^)+(0.0128P)^2^+2.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7806
_reflns_number_total             8285
_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_(100K)
_cod_original_cell_volume        2269.66(5)
_cod_database_code               4135105
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.525
_olex2_refinement_description
;
1. Restrained distances
 O5-H5B
 0.82 with sigma of 0.02
 H5A-O5
 0.82 with sigma of 0.02
;
_shelx_res_checksum              39374
_shelx_hkl_checksum              81015
_olex2_submission_special_instructions 'No special instructions were received'