From a nanoparticular solid-state material to molecular organo-f-element-polyarsenides
Reinfandt, Niklas; Hauser, Adrian; Münzfeld, Luca; Roesky, Peter W.; Chemical Science  (2022) –; doi:10.1039/D1SC05797A

data_1566695
_publ_section_title
;
 From a nanoparticular solid-state material to molecular
 organo-f-element-polyarsenides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05797A
_journal_year                    2022
_chemical_formula_moiety
'C56 H108 As14 Ce2 K O6 Si8, C12 H24 K O6, 4(C7 H8)'
_chemical_formula_sum            'C96 H164 As14 Ce2 K2 O12 Si8'
_chemical_formula_weight         3142.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                72.888(10)
_cell_angle_beta                 89.816(11)
_cell_angle_gamma                73.008(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2230(14)
_cell_length_b                   16.579(2)
_cell_length_c                   18.693(3)
_cell_measurement_reflns_used    10555
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      1.41
_cell_volume                     3166.0(8)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.751
_diffrn_measurement_details
;
 378 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.751
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28716
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.751
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.642
_diffrn_reflns_theta_min         2.273
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.531
_exptl_absorpt_correction_T_max  0.6063
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         16017
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0604P)^2^+6.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1279
_reflns_d_resolution_high        0.677
_reflns_d_resolution_low         8.959
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                11474
_reflns_number_total             16017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nr133r
_cod_original_cell_volume        3165.8(8)
_cod_database_code               1566695
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.372
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C38A \\sim C39A \\sim C40A \\sim C41A \\sim C36A \\sim C37A: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
C40B \\sim C41B \\sim C36B \\sim C37B \\sim C38B \\sim C39B: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
C32A \\sim C28A \\sim O4A \\sim O2A \\sim O5A \\sim O1A \\sim C31A \\sim C30A
\\sim C34A \\sim C26A \\sim C25A \\sim C29A \\sim C23A \\sim C24A \\sim O3A
\\sim O6A \\sim C33A \\sim C27A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
K1A \\sim O3B \\sim C25B \\sim O2B \\sim C29B \\sim O6B \\sim O1B \\sim O4B
\\sim O5B \\sim C23B \\sim C24B \\sim C28B \\sim C32B \\sim C34B \\sim C33B
\\sim C26B \\sim C31B \\sim C27B \\sim C30B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: K1B(0.5) K1A(0.5) C38A(0.5) H38A(0.5) C39A(0.5) H39A(0.5)
 C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) C36A(0.5) C37A(0.5) H37A(0.5)
 C40B(0.5) H40B(0.5) C41B(0.5) H41B(0.5) C36B(0.5) C37B(0.5) H37B(0.5)
 C38B(0.5) H38B(0.5) C39B(0.5) H39B(0.5) O3B(0.5) C25B(0.5) H25A(0.5) H25B(0.5)
 O2B(0.5) C32A(0.5) H32C(0.5) H32D(0.5) C28A(0.5) H28C(0.5) H28D(0.5) C29B(0.5)
 H29A(0.5) H29B(0.5) O6B(0.5) O1B(0.5) O4B(0.5) O4A(0.5) O5B(0.5) O2A(0.5)
 O5A(0.5) C23B(0.5) H23A(0.5) H23B(0.5) O1A(0.5) C47A(0.5) H47A(0.5) C48A(0.5)
 H48A(0.5) C43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45A(0.5) C46A(0.5)
 H46A(0.5) C24B(0.5) H24A(0.5) H24B(0.5) O3A(0.5) C28B(0.5) H28A(0.5) H28B(0.5)
 C32B(0.5) H32A(0.5) H32B(0.5) O6A(0.5) C35A(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 C34B(0.5) H34A(0.5) H34B(0.5) C33B(0.5) H33A(0.5) H33B(0.5) C42A(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C42B(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
 C31A(0.5) H31C(0.5) H31D(0.5) C26B(0.5) H26A(0.5) H26B(0.5) C35B(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5) C46B(0.5) H46B(0.5) C45B(0.5) H45B(0.5)
 C44B(0.5) H44B(0.5) C43B(0.5) C48B(0.5) H48B(0.5) C47B(0.5) H47B(0.5)
 C33A(0.5) H33C(0.5) H33D(0.5) C30A(0.5) H30C(0.5) H30D(0.5) C31B(0.5)
 H31A(0.5) H31B(0.5) C34A(0.5) H34C(0.5) H34D(0.5) C27A(0.5) H27C(0.5)
 H27D(0.5) C26A(0.5) H26C(0.5) H26D(0.5) C25A(0.5) H25C(0.5) H25D(0.5)
 C29A(0.5) H29C(0.5) H29D(0.5) C27B(0.5) H27A(0.5) H27B(0.5) C30B(0.5)
 H30A(0.5) H30B(0.5) C23A(0.5) H23C(0.5) H23D(0.5) C24A(0.5) H24C(0.5) H24D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C25B(H25A,H25B), C32A(H32C,H32D), C28A(H28C,H28D), C29B(H29A,H29B), C23B(H23A,
 H23B), C24B(H24A,H24B), C28B(H28A,H28B), C32B(H32A,H32B), C34B(H34A,H34B),
 C33B(H33A,H33B), C31A(H31C,H31D), C26B(H26A,H26B), C33A(H33C,H33D), C30A(H30C,
 H30D), C31B(H31A,H31B), C34A(H34C,H34D), C27A(H27C,H27D), C26A(H26C,H26D),
 C25A(H25C,H25D), C29A(H29C,H29D), C27B(H27A,H27B), C30B(H30A,H30B), C23A(H23C,
 H23D), C24A(H24C,H24D)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C13(H13), C5(H5), C3(H3), C15(H15), C2(H2), C38A(H38A), C39A(H39A),
 C40A(H40A), C41A(H41A), C37A(H37A), C40B(H40B), C41B(H41B), C37B(H37B),
 C38B(H38B), C39B(H39B), C47A(H47A), C48A(H48A), C44A(H44A), C45A(H45A),
 C46A(H46A), C46B(H46B), C45B(H45B), C44B(H44B), C48B(H48B), C47B(H47B)
4.c Fitted hexagon refined as free rotating group:
 C38A(C39A,C40A,C41A,C36A,C37A), C40B(C41B,C36B,C37B,C38B,C39B), C47A(C48A,
 C43A,C44A,C45A,C46A), C46B(C45B,C44B,C43B,C48B,C47B)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C7(H7A,H7B,
 H7C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C6(H6A,H6B,
 H6C), C35A(H35A,H35B,H35C), C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F),
 C35B(H35D,H35E,H35F)
;
_shelx_res_checksum              8384
_shelx_hkl_checksum              3464
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'