Metal-Induced C‒N Bond Cleavage in the Decomposition of Alkali (R,R)-Bis(α-methylbenzyl)amide Complexes
Border, Emily C.; Maguire, Melissa; MacLellan, Jonathan G.; Andrews, Philip C.; Organometallics 36 (2017) 1496–; doi:10.1021/acs.organomet.7b00074

data_4089240
_publ_section_title
;
 Metal-Induced C--N Bond Cleavage in the Decomposition of Alkali
 (R,R)-Bis(\a-methylbenzyl)amide Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1496
_journal_paper_doi               10.1021/acs.organomet.7b00074
_journal_volume                  36
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C44 H72 Li2 N8 O2 P2'
_chemical_formula_sum            'C44 H72 Li2 N8 O2 P2'
_chemical_formula_weight         820.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0729(9)
_cell_length_b                   27.9462(16)
_cell_length_c                   10.8469(5)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.38
_cell_volume                     4872.2(5)
_computing_cell_refinement       'Bruker Apex2 v2014.1-7 (Bruker AXS, 2014)'
_computing_data_collection       'Bruker Apex2 v2014.1-7 (Bruker AXS, 2014)'
_computing_data_reduction        'Bruker Apex2 v2014.1-7 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/3 (Bruker AXS, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 2698 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0902
_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^)+18.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.1990
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7714
_reflns_number_total             8756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00074_si_002.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               4089240
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              53644
_shelx_hkl_checksum              57091