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_1566698
_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         'C52 H96 As7 K2 Nd O12 Si4, C6 H6'
_chemical_formula_sum            'C58 H102 As7 K2 Nd O12 Si4'
_chemical_formula_weight         1850.63
_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
_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                90
_cell_angle_beta                 98.6780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2709(2)
_cell_length_b                   31.9950(6)
_cell_length_c                   17.4941(3)
_cell_measurement_reflns_used    81775
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.24
_cell_volume                     7896.3(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details
;
 1160 frames, detector distance = 100 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  0.0296
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57719
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.104
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.784
_exptl_absorpt_correction_T_max  0.5463
_exptl_absorpt_correction_T_min  0.2022
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3724
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.142
_refine_diff_density_max         3.375
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         18080
_refine_ls_number_restraints     936
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0635P)^2^+72.4491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.1949
_reflns_d_resolution_high        0.731
_reflns_d_resolution_low         8.647
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              16
_reflns_limit_h_min              -18
_reflns_limit_k_max              39
_reflns_limit_k_min              -42
_reflns_limit_l_max              22
_reflns_limit_l_min              -23
_reflns_number_gt                15489
_reflns_number_total             18080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nr115
_cod_database_code               1566698
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.353
_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. Restrained distances
 O11A-C43A = O11A-C42A = O12A-C44A = O12A-C45A = O7A-C46A = O8A-C36A = O8A-
 C37A = O9A-C39A = O9A-C38A = O10A-C41A
 1.43 with sigma of 0.02
 O7A-C35A = O10A-C40A
 1.42 with sigma of 0.02
 C43A-C44A = C45A-C46A = C35A-C36A = C37A-C38A = C39A-C40A = C41A-C42A
 1.49 with sigma of 0.02
 O12B-C44B = O9B-C39B
 1.42 with sigma of 0.02
 O8B-C36B = O8B-C37B = O7B-C35B = O7B-C46B = O12B-C45B = O11B-C43B = O11B-C42B
 = O10B-C40B = O10B-C41B = O9B-C38B
 1.43 with sigma of 0.02
 C36B-C35B = C46B-C45B = C44B-C43B = C42B-C41B = C40B-C39B = C38B-C37B
 1.49 with sigma of 0.02
 O7A-C45A = O7A-C36A = O8A-C38A
 2.38 with sigma of 0.04
 O11A-C44A = O11A-C41A = O12A-C43A = O12A-C46A = O8A-C35A = O9A-C40A = O10A-
 C42A = O10A-C39A
 2.37 with sigma of 0.04
 O9A-C37A
 2.36 with sigma of 0.04
 O8B-C35B = O8B-C38B = O7B-C36B = O7B-C45B = O11B-C44B = O10B-C39B = O9B-C37B =
  O9B-C40B
 2.37 with sigma of 0.04
 O10B-C42B
 2.36 with sigma of 0.04
 O12B-C46B = O12B-C43B = O11B-C41B
 2.38 with sigma of 0.04
 O11A-C44A \\sim O12A-C46A \\sim O7A-C36A \\sim O8A-C38A \\sim O9A-C40A \\sim
O10A-C42A \\sim O12A-
 C43A \\sim O7A-C45A \\sim O8A-C35A \\sim O9A-C37A \\sim O10A-C39A \\sim
O11A-C41A
 with sigma of 0.04
 O11A-C43A \\sim O11A-C42A \\sim O12A-C44A \\sim O12A-C45A \\sim O7A-C46A \\sim
O7A-C35A \\sim O8A-
 C36A \\sim O8A-C37A \\sim O9A-C38A \\sim O9A-C39A \\sim O10A-C40A \\sim
O10A-C41A
 with sigma of 0.02
 C43A-C44A \\sim C45A-C46A \\sim C35A-C36A \\sim C37A-C38A \\sim C39A-C40A
\\sim C41A-C42A
 with sigma of 0.02
 C44A-C45A \\sim C46A-C35A \\sim C36A-C37A \\sim C38A-C39A \\sim C40A-C41A
\\sim C42A-C43A
 with sigma of 0.04
 O8B-C36B \\sim O8B-C37B \\sim O7B-C35B \\sim O7B-C46B \\sim O12B-C45B \\sim
O12B-C44B \\sim O11B-C43B
 \\sim O11B-C42B \\sim O10B-C41B \\sim O10B-C40B \\sim O9B-C39B \\sim O9B-C38B
 with sigma of 0.02
 C36B-C35B \\sim C46B-C45B \\sim C44B-C43B \\sim C42B-C41B \\sim C40B-C39B
\\sim C38B-C37B
 with sigma of 0.02
 C35B-C46B \\sim C45B-C44B \\sim C43B-C42B \\sim C41B-C40B \\sim C39B-C38B
\\sim C37B-C36B
 with sigma of 0.04
 O8B-C35B \\sim O7B-C45B \\sim O12B-C43B \\sim O11B-C41B \\sim O10B-C39B \\sim
O9B-C37B \\sim O7B-C36B
 \\sim O12B-C46B \\sim O11B-C44B \\sim O10B-C42B \\sim O9B-C40B \\sim O8B-C38B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O11A \\sim O12A \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim C43A \\sim C44A
\\sim C45A \\sim C46A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A
\\sim C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O8B \\sim O7B \\sim O12B \\sim O11B \\sim O10B \\sim O9B \\sim C36B \\sim C35B
\\sim C46B \\sim C45B \\sim C44B \\sim C43B \\sim C42B \\sim C41B \\sim C40B
\\sim C39B \\sim C38B \\sim C37B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Si1B \\sim C1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Si1A \\sim C1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C7A \\sim Si1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C7B \\sim Si1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C8A \\sim Si1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C6A \\sim Si1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C6B \\sim Si1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C8B \\sim Si1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Rigid body (RIGU) restrains
 O11A, O12A, O7A, O8A, O9A, O10A, C43A, C44A, C45A, C46A, C35A, C36A, C37A,
 C38A, C39A, C40A, C41A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8B, O7B, O12B, O11B, O10B, O9B, C36B, C35B, C46B, C45B, C44B, C43B, C42B,
 C41B, C40B, C39B, C38B, C37B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C51, C50, C49, C48, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C58, C57, C56, C55, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: Si1B(0.4) C8B(0.4) H8BA(0.4) H8BB(0.4) H8BC(0.4) C7A(0.6)
 H7AA(0.6) H7AB(0.6) H7AC(0.6) C6A(0.6) H6AA(0.6) H6AB(0.6) H6AC(0.6) O11A(0.6)
 O12A(0.6) O7A(0.6) O8A(0.6) O9A(0.6) O10A(0.6) C43A(0.6) H43A(0.6) H43B(0.6)
 C44A(0.6) H44A(0.6) H44B(0.6) C45A(0.6) H45A(0.6) H45B(0.6) C46A(0.6)
 H46A(0.6) H46B(0.6) C35A(0.6) H35A(0.6) H35B(0.6) C36A(0.6) H36A(0.6)
 H36B(0.6) C37A(0.6) H37A(0.6) H37B(0.6) C38A(0.6) H38A(0.6) H38B(0.6)
 C39A(0.6) H39A(0.6) H39B(0.6) C40A(0.6) H40A(0.6) H40B(0.6) C41A(0.6)
 H41A(0.6) H41B(0.6) C42A(0.6) H42A(0.6) H42B(0.6) O8B(0.4) O7B(0.4) O12B(0.4)
 O11B(0.4) O10B(0.4) O9B(0.4) C36B(0.4) H36C(0.4) H36D(0.4) C35B(0.4) H35C(0.4)
 H35D(0.4) C46B(0.4) H46C(0.4) H46D(0.4) C45B(0.4) H45C(0.4) H45D(0.4)
 C44B(0.4) H44C(0.4) H44D(0.4) C43B(0.4) H43C(0.4) H43D(0.4) C42B(0.4)
 H42C(0.4) H42D(0.4) C41B(0.4) H41C(0.4) H41D(0.4) C40B(0.4) H40C(0.4)
 H40D(0.4) C39B(0.4) H39C(0.4) H39D(0.4) C38B(0.4) H38C(0.4) H38D(0.4)
 C37B(0.4) H37C(0.4) H37D(0.4) C7B(0.4) H7BA(0.4) H7BB(0.4) H7BC(0.4) C6B(0.4)
 H6BA(0.4) H6BB(0.4) H6BC(0.4) Si1A(0.6) C8A(0.6) H8AA(0.6) H8AB(0.6) H8AC(0.6)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B), C32(H32A,H32B), C27(H27A,
 H27B), C28(H28A,H28B), C30(H30A,H30B), C29(H29A,H29B), C31(H31A,H31B),
 C33(H33A,H33B), C34(H34A,H34B), C24(H24A,H24B), C43A(H43A,H43B), C44A(H44A,
 H44B), C45A(H45A,H45B), C46A(H46A,H46B), C35A(H35A,H35B), C36A(H36A,H36B),
 C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B), C41A(H41A,
 H41B), C42A(H42A,H42B), C36B(H36C,H36D), C35B(H35C,H35D), C46B(H46C,H46D),
 C45B(H45C,H45D), C44B(H44C,H44D), C43B(H43C,H43D), C42B(H42C,H42D), C41B(H41C,
 H41D), C40B(H40C,H40D), C39B(H39C,H39D), C38B(H38C,H38D), C37B(H37C,H37D)
6.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C5(H5), C3(H3), C2(H2), C16(H16), C53(H53), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52)
6.c Fitted hexagon refined as free rotating group:
 C53(C54,C55,C56,C57,C58), C47(C48,C49,C50,C51,C52)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C8B(H8BA,
 H8BB,H8BC), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C7A(H7AA,H7AB,H7AC),
 C6A(H6AA,H6AB,H6AC), C7B(H7BA,H7BB,H7BC), C6B(H6BA,H6BB,H6BC), C8A(H8AA,H8AB,
 H8AC)
;
_shelx_res_checksum              20332
_shelx_hkl_checksum              76613
_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'