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_4134512
_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         '0.07(F42 Mo14 O28), N'
_chemical_formula_sum            'F3 Mo N O2'
_chemical_formula_weight         198.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_date             2019-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            28
_cell_length_a                   8.47740(10)
_cell_length_b                   13.39660(10)
_cell_length_c                   28.4385(3)
_cell_measurement_reflns_used    30600
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      38.1520
_cell_measurement_theta_min      2.1720
_cell_volume                     3217.06(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_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    -60.00 -23.00   0.50    1.25    --  -25.33 102.00  39.00   74
  2  \w    -48.00  12.00   0.50    1.25    --   24.71 -37.00  30.00  120
  3  \w    -48.00  -4.00   0.50    1.25    --  -25.33 -77.00 -60.00   88
  4  \w    -98.00  -4.00   0.50    1.25    --  -25.33 -77.00   0.00  188
  5  \w    -98.00 -56.00   0.50    1.25    --  -25.33 -77.00 -60.00   84
  6  \w    -98.00 -13.00   0.50    1.25    --  -25.33 -19.00-180.00  170
  7  \w     42.00  67.00   0.50    1.25    --   24.71 178.00 -90.00   50
  8  \w    -49.00   5.00   0.50    1.25    --   24.71 -19.00 -30.00  108
  9  \w     -6.00  46.00   0.50    1.25    --   24.71 -99.00 120.00  104
 10  \w     72.00  97.00   0.50    1.25    --   24.71-178.00  60.00   50
 11  \w     40.00  66.00   0.50    1.25    --   24.71-178.00  60.00   52
 12  \w    -14.00  53.00   0.50    1.25    --   24.71-102.00 -63.00  134
 13  \w    -83.00 -43.00   0.50    1.25    --  -25.33-178.00  90.00   80
 14  \w    -82.00 -51.00   0.50    1.25    --  -25.33-178.00-150.00   62
;
_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      0.0247768000
_diffrn_orient_matrix_UB_12      0.0495231000
_diffrn_orient_matrix_UB_13      -0.0042162000
_diffrn_orient_matrix_UB_21      0.0758269000
_diffrn_orient_matrix_UB_22      -0.0108849000
_diffrn_orient_matrix_UB_23      0.0114212000
_diffrn_orient_matrix_UB_31      0.0262934000
_diffrn_orient_matrix_UB_32      -0.0152279000
_diffrn_orient_matrix_UB_33      -0.0218860000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            46287
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.229
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   gaussian
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.875
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00211(4)
_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   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         8446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0196P)^2^+5.0977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7998
_reflns_number_total             8446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01218_si_003.cif
_cod_data_source_block           jch_nh4moo2f3_200k
_cod_depositor_comments
'Adding full bibliography for 4134508--4134512.cif.'
_cod_database_code               4134512
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'N H4 Mo O2 F3'
_chemical_oxdiff_usercomment     'clear blocl'
_diffrn_oxdiff_digest_frames
;
01f77d3b317cc3245932e75d2189a1720f0136401f0
;
_diffrn_oxdiff_digest_hkl
;
01b8ffdaafb5c32b2e4b5d2fd89d15173b38f9
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
;
_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 1.237
_oxdiff_exptl_absorpt_empirical_full_min 0.866