0D and 2D: The Cases of Phenylethylammonium Tin Bromide Hybrids
Xu, Liang-Jin; Lin, Haoran; Lee, Sujin; Zhou, Chenkun; Worku, Michael; Chaaban, Maya; He, Qingquan; Plaviak, Anna; Lin, Xinsong; Chen, Banghao; Du, Mao-Hua; Ma, Biwu; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01254

data_4003559
_publ_section_title
;
 0D and 2D: The Cases of Phenylethylammonium Tin Bromide Hybrids
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01254
_journal_year                    2020
_chemical_formula_moiety
'Br3 Sn, 5(Br), 6(C8 H12 N), C0.603 H2 Cl1.206, C0.35 Cl0.768, 0.397(C Cl2), C0.65 H2 Cl1.232'
_chemical_formula_sum            'C50 H76 Br8 Cl4 N6 Sn'
_chemical_formula_weight         1661.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.131(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0550(6)
_cell_length_b                   10.0193(3)
_cell_length_c                   37.8344(14)
_cell_measurement_reflns_used    16560
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      31.3210
_cell_measurement_theta_min      2.3560
_cell_volume                     6343.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.787
_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    -15.00  30.00   0.50   18.53    --    4.56 -85.00 -79.00   90
  2  \w    -31.00  -5.00   0.50   18.53    --   -5.65 -85.00 -79.00   52
  3  \w    -65.00   4.00   0.50   18.53    --    4.56 -19.00  30.00  138
  4  \w    -16.00   9.00   0.50   18.53    --   -5.65 -99.00  60.00   50
  5  \w    -17.00  27.00   0.50   18.53    --   -5.65 -99.00  90.00   88
  6  \w    -22.00  21.00   0.50   18.53    --   -5.65 -99.00 150.00   86
  7  \w    -17.00   8.00   0.50   18.53    --   -5.65  85.00  39.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220299000
_diffrn_orient_matrix_UB_12      0.0589968000
_diffrn_orient_matrix_UB_13      -0.0015964000
_diffrn_orient_matrix_UB_21      0.0298916000
_diffrn_orient_matrix_UB_22      -0.0211114000
_diffrn_orient_matrix_UB_23      0.0146486000
_diffrn_orient_matrix_UB_31      0.0203483000
_diffrn_orient_matrix_UB_32      -0.0330302000
_diffrn_orient_matrix_UB_33      -0.0121574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            25940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.306
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.648
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 6954 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         16371
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0206P)^2^+4.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                15041
_reflns_number_total             16371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01254_si_002.cif
_cod_data_source_block           pea-snbr-1
_cod_database_code               4003559
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SnBr8N6C64H76
_chemical_oxdiff_usercomment     'colorless,hexanol  like, 100K '
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.308
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.500(6)
 0.500(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 Cl2-C49 \\sim Cl2A-C49A
 with sigma of 0.02
 Cl1-C49 \\sim Cl1A-C49A
 with sigma of 0.02
 Cl2-Cl1 \\sim Cl2A-Cl1A
 with sigma of 0.04
 Cl3-Cl4 \\sim Cl3A-Cl4A
 with sigma of 0.04
4. Others
 Sof(C49A)=Sof(Cl2A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl1)=Sof(C49)=FVAR(1)
 Sof(Cl3A)=Sof(Cl4A)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=FVAR(2)
 Fixed Sof: C50(0.65) C51(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C25(H25A,H25B), C10(H10A,H10B), C1(H1D,H1E), C17(H17A,H17B),
 C9(H9A,H9B), C34(H34A,H34B), C33(H33A,H33B), C42(H42A,H42B), C2(H2A,H2B),
 C26(H26A,H26B), C18(H18A,H18B), C49(H49A,H49B), C50(H50A,H50B)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C4(H4), C44(H44), C32(H32), C20(H20), C46(H46), C45(H45), C8(H8),
 C12(H12), C6(H6), C15(H15), C24(H24), C13(H13), C38(H38), C39(H39), C48(H48),
 C40(H40), C30(H30), C28(H28), C5(H5), C47(H47), C14(H14), C29(H29), C36(H36),
 C22(H22), C21(H21), C31(H31), C23(H23), C37(H37), C7(H7)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N5(H5A,H5B,H5C), N6(H6A,
 H6B,H6C), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              76140
_shelx_hkl_checksum              44693
_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 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.577