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_7045113
_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_absolute_configuration rmad
_chemical_formula_moiety
'0.6(C32 H47 As Li N O2), 0.4(C32 H45 As Li N O2)'
_chemical_formula_sum            'C32 H46.2 As Li N O2'
_chemical_formula_weight         558.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-20
_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                90
_cell_angle_beta                 109.809(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7629(4)
_cell_length_b                   16.3472(4)
_cell_length_c                   10.4418(4)
_cell_measurement_reflns_used    27047
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.07
_cell_volume                     1567.86(10)
_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      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  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  0.0786
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.220
_diffrn_reflns_theta_min         2.073
_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    1.11
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.7892
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.570
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.008(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                5655
_reflns_number_total             8466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04401a2.cif
_cod_data_source_block           xcd023
_cod_depositor_comments
'Adding full bibliography for 7045111--7045113.cif.'
_cod_original_formula_sum        'C32 H46.20 As Li N O2'
_cod_database_code               7045113
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.693
_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
 C30B-C31B
 1.5 with sigma of 0.02
 C31A-C32A \\sim C29A-C30A
 with sigma of 0.02
 C32B-C31B \\sim C29B-C30B
 with sigma of 0.02
 C29B-O2B \\sim O2B-C32B
 with sigma of 0.02
 C31A-O2A \\sim O2A-C29A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N \\sim C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim Li: within
1.7A with sigma of 0.002 and sigma for terminal atoms of 0.004
N \\sim C1A \\sim C1AA \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim Li: within
1.7A with sigma of 0.002 and sigma for terminal atoms of 0.004
O2B \\sim C29B \\sim C30B \\sim C31B \\sim C32B: within 1.7A with sigma of
0.002 and sigma for terminal atoms of 0.004
As \\sim O1 \\sim O2B \\sim N \\sim Li: within 1.7A with sigma of 0.002 and
sigma for terminal atoms of 0.004
O2A \\sim C29A \\sim C30A \\sim C31A \\sim C32A: within 1.7A with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(O2A) = Uanis(O2B)
4. Others
 Fixed Sof: O2A(0.6) O2B(0.4) C1A(0.6) C2A(0.6) H2A(0.6) C3A(0.6) H3A(0.6)
 C1AA(0.6) H1AA(0.6) C4A(0.6) H4A(0.6) C5A(0.6) H5A(0.6) C1B(0.4) C2B(0.4)
 H2B(0.4) C3B(0.4) H3B(0.4) C4B(0.4) H4B(0.4) C5B(0.4) H5B(0.4) C6B(0.4)
 H6B(0.4) C29A(0.6) H29A(0.6) H29B(0.6) C29B(0.4) H29C(0.4) H29D(0.4) C30A(0.6)
 H30A(0.6) H30B(0.6) H30C(0.6) C30B(0.4) H30D(0.4) H30E(0.4) C31A(0.6)
 H31A(0.6) H31B(0.6) C31B(0.4) H31C(0.4) H31D(0.4) C32A(0.6) H32A(0.6)
 H32B(0.6) H32C(0.6) C32B(0.4) H32D(0.4) H32E(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C27(H27A,H27B), C29A(H29A,H29B), C29B(H29C,H29D), C30B(H30D,
 H30E), C31A(H31A,H31B), C31B(H31C,H31D), C32B(H32D,H32E)
5.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C1AA(H1AA), C4A(H4A), C5A(H5A), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C9(H9), C11(H11), C18(H18), C20(H20)
5.c Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C1AA,C4A,C5A), C1B(C2B,C3B,C4B,C5B,C6B)
5.d 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), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C)
;
_shelx_res_checksum              47648
_olex2_submission_special_instructions 'No special instructions were received'