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_7045112
_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 H70 As2 K2 N2 O2'
_chemical_formula_sum            'C56 H70 As2 K2 N2 O2'
_chemical_formula_weight         1031.18
_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'
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_audit_update_record
;
2017-11-20 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.450(4)
_cell_angle_beta                 81.984(4)
_cell_angle_gamma                76.104(4)
_cell_formula_units_Z            1
_cell_length_a                   9.7359(5)
_cell_length_b                   10.7675(6)
_cell_length_c                   14.0129(7)
_cell_measurement_reflns_used    15022
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      1.58
_cell_volume                     1315.14(13)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
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_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
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X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.70.0.0 (STOE, 2017)
PLATON (A.L.Spek, 2009)
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_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
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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)
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_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
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_diffrn_ambient_temperature      210
_diffrn_detector                 'image plate (34cm diameter)'
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_diffrn_measured_fraction_theta_full 0.991
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_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_max       19
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_diffrn_reflns_number            13130
_diffrn_reflns_point_group_measured_fraction_full 0.991
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_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
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_diffrn_source_power             2kW
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_exptl_absorpt_coefficient_mu    1.47
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;
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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.111
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_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_R_factor_all          0.0805
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.9213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                5097
_reflns_number_total             7205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04401a2.cif
_cod_data_source_block           xcd11
_cod_depositor_comments
'Adding full bibliography for 7045111--7045113.cif.'
_cod_database_code               7045112
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.854
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_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:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              79048
_olex2_submission_special_instructions 'No special instructions were received'