Aminotroponiminates: Alkali Metal Compounds Reveal Unprecedented Coordination Modes
Lichtenberg, Crispin; Organometallics 35 (2016) 894–; doi:10.1021/acs.organomet.6b00042

data_4086434
_publ_section_title
;
 Aminotroponiminates: Alkali Metal Compounds Reveal Unprecedented
 Coordination Modes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              894
_journal_paper_doi               10.1021/acs.organomet.6b00042
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C38 H40 Li N2 O2 P, C7 H8'
_chemical_formula_sum            'C45 H48 Li N2 O2 P'
_chemical_formula_weight         686.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5767(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3602(5)
_cell_length_b                   10.5422(5)
_cell_length_c                   31.8629(16)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    100.6
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.32
_cell_volume                     3773.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            68660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_min         2.325
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0525 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.9527.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10590
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0580P)^2^+1.6280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8367
_reflns_number_total             10590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00042_si_002.cif
_cod_data_source_block           2-thf-OPPh3
_cod_depositor_comments
'Adding full bibliography for 4086434--4086438.cif.'
_cod_database_code               4086434
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.946
_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
 H7-H8
 2.03 with sigma of 0.001
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C38(H38A,H38B), C36(H36A,H36B), C37(H37A,H37B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C28(H28), C4(H4), C7(H7), C34(H34), C25(H25), C16(H16), C15(H15),
 C24(H24), C5(H5), C3(H3), C30(H30), C12(H12), C26(H26), C18(H18), C22(H22),
 C32(H32), C33(H33), C27(H27), C43(H43), C40(H40), C31(H31), C14(H14), C19(H19),
  C44(H44), C13(H13), C41(H41), C42(H42), C20(H20), C21(H21)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              86061
_shelx_hkl_checksum              62888
_olex2_submission_special_instructions 'No special instructions were received'