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_1566700
_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
'C62 H120 As14 K1.5 Nd2 O9 Si8, 0.5(C12 H24 K O6), C6 H6'
_chemical_formula_sum            'C74 H138 As14 K2 Nd2 O12 Si8'
_chemical_formula_weight         2860.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-14 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.516(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.5910(16)
_cell_length_b                   13.2497(4)
_cell_length_c                   19.5306(8)
_cell_measurement_reflns_used    19893
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.18
_cell_measurement_theta_min      2.10
_cell_volume                     10712.9(7)
_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      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details
;
 326 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28105
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.324
_diffrn_reflns_theta_min         2.095
_exptl_absorpt_coefficient_mu    5.466
_exptl_absorpt_correction_T_max  0.7809
_exptl_absorpt_correction_T_min  0.3902
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         13590
_refine_ls_number_restraints     378
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0625P)^2^+7.3484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8536
_reflns_number_total             13590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nrndasn60
_cod_database_code               1566700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.587
_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
 C30A-C29A \\sim C32A-C31A \\sim C34A-C33A \\sim C24A-C23A \\sim C26A-C25A
\\sim C28A-C27A
 with sigma of 0.01
 O1A-C34A \\sim O1A-C23A \\sim O2A-C24A \\sim O2A-C25A \\sim O3A-C26A \\sim
O3A-C27A \\sim O4A-C28A ~
 O4A-C29A \\sim O5A-C30A \\sim O5A-C31A \\sim O6A-C32A \\sim O6A-C33A
 with sigma of 0.01
 C23B-C24B \\sim C34B-C33B \\sim C31B-C32B \\sim C29B-C30B \\sim C27B-C28B
\\sim C26B-C25B
 with sigma of 0.01
 O6B-C33B \\sim O1B-C34B \\sim O2B-C24B \\sim O1B-C23B \\sim O2B-C25B \\sim
O3B-C26B \\sim O3B-C27B ~
 O4B-C28B \\sim O4B-C29B \\sim O5B-C30B \\sim O5B-C31B \\sim O6B-C32B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33A \\sim C23A \\sim C32A \\sim C34A \\sim C25A \\sim C27A \\sim O3A \\sim
C26A \\sim O2A \\sim O1A \\sim O5A \\sim O6A \\sim C31A \\sim O4A \\sim C28A
\\sim C29A \\sim C30A \\sim C24A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O1B \\sim O2B \\sim C24B \\sim C25B \\sim C33B \\sim C26B \\sim O5B \\sim C23B
\\sim C32B \\sim C31B \\sim C34B \\sim O6B \\sim C30B \\sim O4B \\sim C29B
\\sim C28B \\sim C27B \\sim O3B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: K1A(0.75) O1B(0.25) O2B(0.25) C33A(0.75) H33A(0.75) H33B(0.75)
 C23A(0.75) H23A(0.75) H23B(0.75) C24B(0.25) H24C(0.25) H24D(0.25) C32A(0.75)
 H32A(0.75) H32B(0.75) C34A(0.75) H34A(0.75) H34B(0.75) C25A(0.75) H25A(0.75)
 H25B(0.75) C25B(0.25) H25C(0.25) H25D(0.25) C27A(0.75) H27A(0.75) H27B(0.75)
 O3A(0.75) C26A(0.75) H26A(0.75) H26B(0.75) K1B(0.25) C33B(0.25) H33C(0.25)
 H33D(0.25) O2A(0.75) C26B(0.25) H26C(0.25) H26D(0.25) O5B(0.25) O1A(0.75)
 O5A(0.75) C23B(0.25) H23C(0.25) H23D(0.25) C32B(0.25) H32C(0.25) H32D(0.25)
 C31B(0.25) H31C(0.25) H31D(0.25) C34B(0.25) H34C(0.25) H34D(0.25) O6A(0.75)
 O6B(0.25) C31A(0.75) H31A(0.75) H31B(0.75) O4A(0.75) C28A(0.75) H28A(0.75)
 H28B(0.75) C29A(0.75) H29A(0.75) H29B(0.75) C30A(0.75) H30A(0.75) H30B(0.75)
 C30B(0.25) H30C(0.25) H30D(0.25) O4B(0.25) C29B(0.25) H29C(0.25) H29D(0.25)
 C24A(0.75) H24A(0.75) H24B(0.75) C28B(0.25) H28C(0.25) H28D(0.25) C27B(0.25)
 H27C(0.25) H27D(0.25) O3B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C33A(H33A,H33B), C23A(H23A,H23B), C24B(H24C,H24D), C32A(H32A,H32B), C34A(H34A,
 H34B), C25A(H25A,H25B), C25B(H25C,H25D), C27A(H27A,H27B), C26A(H26A,H26B),
 C33B(H33C,H33D), C26B(H26C,H26D), C23B(H23C,H23D), C32B(H32C,H32D), C31B(H31C,
 H31D), C34B(H34C,H34D), C31A(H31A,H31B), C28A(H28A,H28B), C29A(H29A,H29B),
 C30A(H30A,H30B), C30B(H30C,H30D), C29B(H29C,H29D), C24A(H24A,H24B), C28B(H28C,
 H28D), C27B(H27C,H27D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C43(H43), C30(H30), C16(H16), C15(H15), C36(H36), C37(H37),
 C35(H35)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              9741
_shelx_hkl_checksum              37298
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'