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_1566697
_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
'C44 H84 As3 Nd2 Si8, 2(C6 H12 K0.5 O3), 3.5(C6 H6)'
_chemical_formula_sum            'C77 H129 As3 K Nd2 O6 Si8'
_chemical_formula_weight         1927.85
_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             2021-03-26
_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                84.855(9)
_cell_angle_beta                 79.390(9)
_cell_angle_gamma                71.581(8)
_cell_formula_units_Z            2
_cell_length_a                   11.7764(13)
_cell_length_b                   17.4676(14)
_cell_length_c                   26.292(4)
_cell_measurement_reflns_used    60034
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      1.44
_cell_volume                     5040.7(11)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_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      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
 321 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47603
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.228
_diffrn_reflns_theta_min         1.438
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  0.7670
_exptl_absorpt_correction_T_min  0.5797
_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    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1978
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.892
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         22194
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+14.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1169
_reflns_d_resolution_high        0.777
_reflns_d_resolution_low         14.179
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              33
_reflns_limit_l_min              -33
_reflns_number_gt                16809
_reflns_number_total             22194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05797a2.cif
_cod_data_source_block           nrndas7-61
_cod_original_cell_volume        5040.6(10)
_cod_database_code               1566697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C20A \\sim Si2: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Si2 \\sim C21A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C79A) \\sim Ueq, Uanis(C78A) \\sim Ueq, Uanis(C77A) \\sim Ueq,
Uanis(C76A) \\sim Ueq, Uanis(C75A) \\sim Ueq, Uanis(C80A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C78B) \\sim Ueq, Uanis(C77B) \\sim Ueq, Uanis(C76B) \\sim Ueq,
Uanis(C75B) \\sim Ueq, Uanis(C80B) \\sim Ueq, Uanis(C79B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74B) \\sim Ueq, Uanis(C69B) \\sim Ueq, Uanis(C71B) \\sim Ueq,
Uanis(C70B) \\sim Ueq, Uanis(C72B) \\sim Ueq, Uanis(C73B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C71A) \\sim Ueq,
Uanis(C72A) \\sim Ueq, Uanis(C73A) \\sim Ueq, Uanis(C74A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O1B(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H46C(0.5) H46D(0.5)
 H46A(0.5) H46B(0.5) C45B(0.5) H45A(0.5) H45B(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 H9C(0.5) C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C47B(0.5) H47A(0.5) H47B(0.5)
 C49B(0.5) H49A(0.5) H49B(0.5) C50B(0.5) H50A(0.5) H50B(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) H10C(0.5) C21B(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) C22B(0.5) H22A(0.5) H22B(0.5) H22C(0.5) Si10(0.5) Si9(0.5)
 C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5)
 C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) Si2(0.5) Si35(0.5) C22A(0.5) H22D(0.5)
 H22E(0.5) H22F(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C21A(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C49A(0.5) H49C(0.5) H49D(0.5) C50A(0.5)
 H50C(0.5) H50D(0.5) C47A(0.5) H47C(0.5) H47D(0.5) C48B(0.5) H48C(0.5)
 H48D(0.5) O1A(0.5) C45A(0.5) H45C(0.5) H45D(0.5) C72A(0.25) H72D(0.25)
 C73A(0.25) H73D(0.25) C74A(0.25) H74D(0.25) C69A(0.25) H69A(0.25) C70A(0.25)
 H70A(0.25) C71A(0.25) H71A(0.25) C76B(0.5) H76B(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) C75A(0.5) H75A(0.5) C80A(0.5) H80A(0.5) C79A(0.5) H79A(0.5)
 C78A(0.5) H78A(0.5) C77A(0.5) H77A(0.5) C76A(0.5) H76A(0.5) C74B(0.25)
 H74E(0.25) C69B(0.25) H69B(0.25) C70B(0.25) H70B(0.25) C71B(0.25) H71B(0.25)
 C72B(0.25) H72E(0.25) C73B(0.25) H73E(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C48A(H48A,H48B), C52(H52A,H52B), C51(H51A,H51B), C56(H56A,
 H56B), C46(H46C,H46D), C46(H46A,H46B), C55(H55A,H55B), C54(H54A,H54B),
 C45B(H45A,H45B), C47B(H47A,H47B), C49B(H49A,H49B), C50B(H50A,H50B), C49A(H49C,
 H49D), C50A(H50C,H50D), C47A(H47C,H47D), C48B(H48C,H48D), C45A(H45C,H45D)
4.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C2(H2), C37(H37), C24(H24), C35(H35), C25(H25), C5(H5), C14(H14),
 C13(H13), C38(H38), C16(H16), C4(H4), C58(H58), C62(H62), C57(H57), C61(H61),
 C59(H59), C60(H60), C72A(H72D), C73A(H73D), C74A(H74D), C69A(H69A), C70A(H70A),
  C71A(H71A), C76B(H76B), C75B(H75B), C80B(H80B), C79B(H79B), C78B(H78B),
 C77B(H77B), C75A(H75A), C80A(H80A), C79A(H79A), C78A(H78A), C77A(H77A),
 C76A(H76A), C68(H68), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
 C74B(H74E), C69B(H69B), C70B(H70B), C71B(H71B), C72B(H72E), C73B(H73E)
4.c Fitted hexagon refined as free rotating group:
 C72A(C73A,C74A,C69A,C70A,C71A), C76B(C75B,C80B,C79B,C78B,C77B), C75A(C80A,
 C79A,C78A,C77A,C76A), C68(C63,C64,C65,C66,C67), C74B(C69B,C70B,C71B,C72B,C73B)
4.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C29(H29A,H29B,
 H29C), C32(H32A,H32B,H32C), C8(H8A,H8B,H8C), C40(H40A,H40B,H40C), C7(H7A,H7B,
 H7C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C39(H39A,
 H39B,H39C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C9(H9A,H9B,H9C),
 C18(H18A,H18B,H18C), C20B(H20A,H20B,H20C), C31(H31A,H31B,H31C), C6(H6A,H6B,
 H6C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C21B(H21A,H21B,H21C), C11(H11A,
 H11B,H11C), C22B(H22A,H22B,H22C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
 C72(H72A,H72B,H72C), C22A(H22D,H22E,H22F), C20A(H20D,H20E,H20F), C21A(H21D,
 H21E,H21F)
;
_shelx_res_checksum              28828
_shelx_hkl_checksum              80756
_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'