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_1566699
_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 Ce2 K O6 Si8, 3(C7 H8)'
_chemical_formula_sum            'C77 H132 As7 Ce2 K O6 Si8'
_chemical_formula_weight         2222.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 96.273(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0117(4)
_cell_length_b                   18.0444(3)
_cell_length_c                   27.5019(6)
_cell_measurement_reflns_used    46357
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.30
_cell_measurement_theta_min      2.05
_cell_volume                     9871.5(3)
_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  'Olex2 1.3 (Dolomanov et al., 2009)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
 398 frames, detector distance = 60 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  0.0327
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            60541
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.288
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.421
_exptl_absorpt_correction_T_max  0.5747
_exptl_absorpt_correction_T_min  0.4060
_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    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.171
_refine_diff_density_max         2.261
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         25742
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0749
_reflns_d_resolution_high        0.705
_reflns_d_resolution_low         10.731
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              27
_reflns_limit_h_min              -23
_reflns_limit_k_max              25
_reflns_limit_k_min              -23
_reflns_limit_l_max              27
_reflns_limit_l_min              -38
_reflns_number_gt                17981
_reflns_number_total             25742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nr133tol
_cod_database_code               1566699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C72A) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C76A) \\sim Ueq,
Uanis(C75A) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(C73A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C74B) \\sim Ueq, Uanis(C75B) \\sim Ueq, Uanis(C76B) \\sim Ueq,
Uanis(C77B) \\sim Ueq, Uanis(C72B) \\sim Ueq, Uanis(C73B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C71A) \\sim Ueq, Uanis(C72A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Fixed Sof: C72A(0.65) C73A(0.65) H73A(0.65) C74A(0.65) H74A(0.65) C75A(0.65)
 H75A(0.65) C76A(0.65) H76A(0.65) C77A(0.65) H77A(0.65) C71A(0.65) H71A(0.65)
 H71B(0.65) H71C(0.65) C71B(0.35) H71D(0.35) H71E(0.35) H71F(0.35) C72B(0.35)
 C73B(0.35) H73B(0.35) C74B(0.35) H74B(0.35) C75B(0.35) H75B(0.35) C76B(0.35)
 H76B(0.35) C77B(0.35) H77B(0.35)
3.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48A,H48B), C55(H55A,H55B), C53(H53A,H53B), C45(H45A,
 H45B), C54(H54A,H54B), C49(H49A,H49B), C50(H50A,H50B), C56(H56A,H56B),
 C46(H46A,H46B), C51(H51A,H51B), C52(H52A,H52B)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C3(H3), C5(H5), C38(H38), C15(H15), C16(H16), C2(H2), C35(H35),
 C25(H25), C13(H13), C37(H37), C27(H27), C63(H63), C62(H62), C59(H59), C61(H61),
  C60(H60), C68(H68), C67(H67), C70(H70), C69(H69), C66(H66), C73A(H73A),
 C74A(H74A), C75A(H75A), C76A(H76A), C77A(H77A), C73B(H73B), C74B(H74B),
 C75B(H75B), C76B(H76B), C77B(H77B)
3.c Fitted hexagon refined as free rotating group:
 C72A(C73A,C74A,C75A,C76A,C77A), C72B(C73B,C74B,C75B,C76B,C77B)
3.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C19(H19A,H19B,H19C), C39(H39A,H39B,
 H39C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C),
 C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C22(H22A,H22B,H22C), C18(H18A,H18B,
 H18C), C17(H17A,H17B,H17C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C31(H31A,
 H31B,H31C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C40(H40A,H40B,
 H40C), C57(H57A,H57B,H57C), C7(H7A,H7B,H7C), C64(H64A,H64B,H64C), C71A(H71A,
 H71B,H71C), C71B(H71D,H71E,H71F)
;
_shelx_res_checksum              30753
_shelx_hkl_checksum              30002
_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'