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

data_4086436
_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_absolute_configuration unk
_chemical_formula_moiety         'C20 H25 K N2 O'
_chemical_formula_sum            'C20 H25 K N2 O'
_chemical_formula_weight         348.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-27
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_length_a                   11.1238(7)
_cell_length_b                   8.0223(5)
_cell_length_c                   21.1968(13)
_cell_measurement_reflns_used    1814
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.1130
_cell_volume                     1838.9(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -91.00  -50.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1405 -179.0000  -90.0000 41

  2 omega   -6.00   52.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1405   57.0000   60.0000 58

  3 omega  -53.00   56.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1405   19.0000 -150.0000 109

  4 omega  -14.00   65.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       15.6093   77.0000  120.0000 79
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_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0141836000
_diffrn_orient_matrix_UB_12      0.0498113000
_diffrn_orient_matrix_UB_13      -0.0284156000
_diffrn_orient_matrix_UB_21      -0.0610438000
_diffrn_orient_matrix_UB_22      -0.0322814000
_diffrn_orient_matrix_UB_23      -0.0077205000
_diffrn_orient_matrix_UB_31      -0.0193655000
_diffrn_orient_matrix_UB_32      0.0655633000
_diffrn_orient_matrix_UB_33      0.0178063000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9090
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         3.119
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2163
_reflns_number_total             3246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00042_si_002.cif
_cod_data_source_block           4-thf
_cod_depositor_comments
'Adding full bibliography for 4086434--4086438.cif.'
_cod_database_code               4086436
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C40H40N2K1O1
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C20(H20A,H20B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C16(H16), C13(H13), C12(H12), C15(H15), C7(H7), C14(H14),
 C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              99389
_shelx_hkl_checksum              45137
_olex2_submission_special_instructions 'No special instructions were received'