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_1566694
_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 As7 K La2 O6 Si8, 4.5(C6 H6)'
_chemical_formula_sum            'C83 H135 As7 K La2 O6 Si8'
_chemical_formula_weight         2294.98
_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             2021-05-20
_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                106.435(3)
_cell_angle_beta                 102.572(3)
_cell_angle_gamma                100.222(3)
_cell_formula_units_Z            2
_cell_length_a                   15.7346(5)
_cell_length_b                   18.2731(6)
_cell_length_c                   19.7473(7)
_cell_measurement_reflns_used    72192
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      1.91
_cell_volume                     5139.0(3)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_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 1.88, Darmstadt 2019
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measurement_details
;
 464 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  0.0401
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55039
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.790
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.594
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.234
_exptl_absorpt_correction_T_max  0.4254
_exptl_absorpt_correction_T_min  0.2472
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2314
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.235
_refine_diff_density_max         4.346
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         27226
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+21.4137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1760
_reflns_d_resolution_high        0.678
_reflns_d_resolution_low         10.564
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              25
_reflns_limit_k_min              -26
_reflns_limit_l_max              26
_reflns_limit_l_min              -25
_reflns_number_gt                19894
_reflns_number_total             27226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           ah133
_cod_database_code               1566694
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.383
_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
C76A \\sim C77A \\sim C78A \\sim C75A \\sim C80A \\sim C79A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C82B \\sim C83B \\sim C84B \\sim C85B \\sim C86B \\sim C81B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C80B \\sim C75B \\sim C76B \\sim C77B \\sim C79B \\sim C78B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C73B \\sim C71B \\sim C72B \\sim C70B \\sim C69B \\sim C74B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C69A \\sim C74A \\sim C73A \\sim C72A \\sim C71A \\sim C70A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C63: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C17 \\sim Si3: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3. Others
 Fixed Sof: C78A(0.5) H78A(0.5) C77A(0.5) H77A(0.5) C76A(0.5) H76A(0.5)
 C75A(0.5) H75A(0.5) C80A(0.5) H80A(0.5) C79A(0.5) H79A(0.5) C84B(0.5)
 H84B(0.5) C83B(0.5) H83B(0.5) C82B(0.5) H82B(0.5) C81B(0.5) H81B(0.5)
 C86B(0.5) H86B(0.5) C85B(0.5) H85B(0.5) C75B(0.5) H75B(0.5) C80B(0.5)
 H80B(0.5) C79B(0.5) H79B(0.5) C78B(0.5) H78B(0.5) C77B(0.5) H77B(0.5)
 C76B(0.5) H76B(0.5) C71B(0.5) H71B(0.5) C72B(0.5) H72B(0.5) C73B(0.5)
 H73B(0.5) C74B(0.5) H74B(0.5) C69B(0.5) H69B(0.5) C70B(0.5) H70B(0.5)
 C72A(0.5) H72A(0.5) C73A(0.5) H73A(0.5) C74A(0.5) H74A(0.5) C69A(0.5)
 H69A(0.5) C70A(0.5) H70A(0.5) C71A(0.5) H71A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C56(H56A,H56B), C53(H53A,H53B), C55(H55A,H55B), C51(H51A,
 H51B), C49(H49A,H49B), C54(H54A,H54B), C52(H52A,H52B), C47(H47A,H47B),
 C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C35(H35), C27(H27), C4(H4), C37(H37), C5(H5), C2(H2), C13(H13),
 C15(H15), C24(H24), C16(H16), C38(H38), C60(H60), C62(H62), C65(H65), C66(H66),
  C67(H67), C68(H68), C63(H63), C64(H64), C61(H61), C57(H57), C58(H58),
 C59(H59), C78A(H78A), C77A(H77A), C76A(H76A), C75A(H75A), C80A(H80A),
 C79A(H79A), C84B(H84B), C83B(H83B), C82B(H82B), C81B(H81B), C86B(H86B),
 C85B(H85B), C75B(H75B), C80B(H80B), C79B(H79B), C78B(H78B), C77B(H77B),
 C76B(H76B), C71B(H71B), C72B(H72B), C73B(H73B), C74B(H74B), C69B(H69B),
 C70B(H70B), C72A(H72A), C73A(H73A), C74A(H74A), C69A(H69A), C70A(H70A),
 C71A(H71A)
4.c Fitted hexagon refined as free rotating group:
 C65(C66,C67,C68,C63,C64), C78A(C77A,C76A,C75A,C80A,C79A), C84B(C83B,C82B,C81B,
 C86B,C85B), C75B(C80B,C79B,C78B,C77B,C76B), C71B(C72B,C73B,C74B,C69B,C70B),
 C72A(C73A,C74A,C69A,C70A,C71A)
4.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C41(H41A,H41B,H41C), C8(H8A,H8B,H8C), C20(H20A,
 H20B,H20C), C7(H7A,H7B,H7C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C),
 C18(H18A,H18B,H18C), C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C10(H10A,H10B,
 H10C), C31(H31A,H31B,H31C), C6(H6A,H6B,H6C), C40(H40A,H40B,H40C), C22(H22A,
 H22B,H22C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C),
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              91817
_shelx_hkl_checksum              16117
_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'