Periodic Tendril Perversion and Helices in the AMoO<sub>2</sub>F<sub>3</sub> (A = K, Rb, NH<sub>4</sub>, Tl) Family.
Hancock, Justin C.; Nisbet, Matthew L.; Zhang, Weiguo; Halasyamani, P. Shiv; Poeppelmeier, Kenneth R.; Journal of the American Chemical Society 142 (2020) 6375–6380; doi:10.1021/jacs.0c01218

data_4134508
_publ_section_title
;
 Periodic Tendril Perversion and Helices in the
 AMoO<sub>2</sub>F<sub>3</sub> (A = K, Rb, NH<sub>4</sub>, Tl) Family.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6375
_journal_page_last               6380
_journal_paper_doi               10.1021/jacs.0c01218
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'F3 Mo O2, K'
_chemical_formula_sum            'F3 K Mo O2'
_chemical_formula_weight         224.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_audit_creation_date             2019-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   11.37930(10)
_cell_length_b                   11.8884(2)
_cell_length_c                   12.7447(2)
_cell_measurement_reflns_used    17800
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      38.2200
_cell_measurement_theta_min      2.3190
_cell_volume                     1724.12(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_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 0.946
_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     30.00  83.00   0.50    0.70    --   24.71-147.00 125.00  106
  2  \w    -84.00 -26.00   0.50    0.70    --  -25.33 147.00 175.00  116
  3  \w    -38.00  47.00   0.50    0.70    --  -25.33  37.00 147.00  170
  4  \w     41.00  93.00   0.50    0.70    --   24.71-178.00 120.00  104
  5  \w    -25.00   5.00   0.50    0.70    --   24.71 -19.00 -90.00   60
  6  \w    -98.00 -44.00   0.50    0.70    --  -25.33 178.00 120.00  108
;
_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      -0.0550022000
_diffrn_orient_matrix_UB_12      -0.0099955000
_diffrn_orient_matrix_UB_13      0.0244575000
_diffrn_orient_matrix_UB_21      0.0289519000
_diffrn_orient_matrix_UB_22      -0.0276154000
_diffrn_orient_matrix_UB_23      0.0420096000
_diffrn_orient_matrix_UB_31      0.0048310000
_diffrn_orient_matrix_UB_32      0.0519561000
_diffrn_orient_matrix_UB_33      0.0270427000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.027
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.962
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.452
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.781
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 3570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(15)
_refine_ls_extinction_coef       0.00165(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         8805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0167P)^2^+0.1464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0463
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                8448
_reflns_number_total             8805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01218_si_006.cif
_cod_data_source_block           jch_kmoof_3
_cod_depositor_comments
'Adding full bibliography for 4134508--4134512.cif.'
_cod_database_code               4134508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K Mo O2 F3'
_diffrn_oxdiff_digest_frames
;
017d1d6c62987cb7a0239abca5070fa9f8006642b7c
;
_diffrn_oxdiff_digest_hkl
;
01abf14578a8079d1673892b90705651cd130d
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
;
_shelx_res_checksum              55351
_shelx_hkl_checksum              62327
_olex2_submission_original_sample_id JCH_KMoOF_3
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.869