Synthesis and structural characterization of alkali metal arsinoamides.
Chen, Xiao; Gamer, Michael T.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12521–12525; doi:10.1039/c7dt04401a

data_7045111
_publ_section_title
;
 Synthesis and structural characterization of alkali metal arsinoamides.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12521
_journal_page_last               12525
_journal_paper_doi               10.1039/c7dt04401a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C56 H74 As2 N2 Na2 O2'
_chemical_formula_sum            'C56 H74 As2 N2 Na2 O2'
_chemical_formula_weight         1002.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-20 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.314(5)
_cell_angle_beta                 75.737(5)
_cell_angle_gamma                69.727(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4020(6)
_cell_length_b                   10.5518(6)
_cell_length_c                   13.2663(8)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      1.58
_cell_volume                     1321.92(14)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.70.0.0 (STOE, 2017)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (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 1.77, Darmstadt 2016
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2017/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.945
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12326
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.567
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current           40mA
_diffrn_source_power             2kW
_diffrn_source_voltage           50kV
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.8905
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_type   integration
_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
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0642P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4646
_reflns_number_total             7012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04401a2.cif
_cod_data_source_block           xcd046
_cod_depositor_comments
'Adding full bibliography for 7045111--7045113.cif.'
_cod_original_cell_volume        1321.93(14)
_cod_database_code               7045111
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.673
_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
 OA-Na \\sim OB-Na
 with sigma of 0.004
 C25B-OB \\sim OB-C27B
 with sigma of 0.004
 C25A-OA \\sim OA-C27A
 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
C25A \\sim C26A \\sim C27A \\sim C28A \\sim OA: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
C25B \\sim C26B \\sim C27B \\sim C28B \\sim OB: within 1.7A with sigma of 0.006
and sigma for terminal atoms of 0.012
4. Others
 Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(OB)=
 1-FVAR(1)
 Sof(OA)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27A(H27A,H27B), C25A(H25A,H25B), C27B(H27C,H27D), C25B(H25C,H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C9(H9), C20(H20), C18(H18)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C28A(H28A,H28B,H28C),
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C28B(H28D,H28E,H28F)
;
_shelx_res_checksum              31450
_olex2_submission_special_instructions 'No special instructions were received'