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_1566696
_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 Nd2 O6 Si8, 4(C6 H6)'
_chemical_formula_sum            'C80 H132 As7 K Nd2 O6 Si8'
_chemical_formula_weight         2266.59
_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
_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                111.299(4)
_cell_angle_beta                 104.839(4)
_cell_angle_gamma                100.119(4)
_cell_formula_units_Z            2
_cell_length_a                   15.6899(7)
_cell_length_b                   18.4469(10)
_cell_length_c                   20.1223(11)
_cell_measurement_reflns_used    67163
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.52
_cell_measurement_theta_min      1.98
_cell_volume                     5006.3(5)
_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 2018/2 (Sheldrick, 2018)'
_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 0.783
_diffrn_measurement_details
;
 424 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  0.0493
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.783
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.667
_diffrn_reflns_theta_min         1.980
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.502
_exptl_absorpt_correction_T_max  0.0703
_exptl_absorpt_correction_T_min  0.0390
_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.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         26464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0883P)^2^+14.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1648
_reflns_d_resolution_high        0.677
_reflns_d_resolution_low         10.288
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              23
_reflns_limit_k_min              -26
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                19574
_reflns_number_total             26464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nrndas7y
_cod_database_code               1566696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.363
_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.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C51(H51A,H51B), C48(H48A,H48B), C55(H55A,H55B), C54(H54A,
 H54B), C49(H49A,H49B), C56(H56A,H56B), C45(H45A,H45B), C47(H47A,H47B),
 C53(H53A,H53B), C50(H50A,H50B), C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C38(H38), C3(H3), C2(H2), C16(H16), C24(H24), C5(H5), C27(H27),
 C25(H25), C35(H35), C14(H14), C36(H36), C69(H69), C74(H74), C70(H70), C62(H62),
  C57(H57), C71(H71), C72(H72), C76(H76), C61(H61), C73(H73), C67(H67),
 C68(H68), C59(H59), C66(H66), C77(H77), C63(H63), C80(H80), C75(H75), C58(H58),
  C79(H79), C78(H78), C64(H64), C65(H65), C60(H60)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C),
 C10(H10A,H10B,H10C), C43(H43A,H43B,H43C), C30(H30A,H30B,H30C), C44(H44A,H44B,
 H44C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C32(H32A,H32B,H32C), C11(H11A,
 H11B,H11C), C40(H40A,H40B,H40C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C9(H9A,
 H9B,H9C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C28(H28A,H28B,
 H28C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              47069
_shelx_hkl_checksum              98906
_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'