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_4135103
_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         'F9 H6 K5 Mo3 O7'
_chemical_formula_sum            'F9 H6 K5 Mo3 O7'
_chemical_formula_weight         772.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1217(3)
_cell_length_b                   7.9281(2)
_cell_length_c                   14.9286(4)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.71
_cell_measurement_theta_min      4.95
_cell_volume                     1539.94(7)
_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
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.761
_diffrn_reflns_theta_min         1.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_T_max  0.7285
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1149 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.8493.
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    3.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00251(15)
_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   1.063
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.6005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4550
_reflns_number_total             4726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04019_si_002.cif
_cod_data_source_block           K5[Mo3O4F9]_3H2O_(100K)
_cod_database_code               4135103
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.505
_olex2_refinement_description
;
;
_shelx_res_checksum              14770
_shelx_hkl_checksum              65670
_olex2_submission_special_instructions 'No special instructions were received'