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

data_4086438
_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         'C39 H37 N6 Na O3 W, 0.5(C5 H12 O), C5 H5 N'
_chemical_formula_sum            'C46.5 H48 N7 Na O3.5 W'
_chemical_formula_weight         967.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   44.458(2)
_cell_length_b                   76.228(4)
_cell_length_c                   10.6621(6)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.37
_cell_volume                     36133(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       94
_diffrn_reflns_limit_k_min       -99
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            64808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.717
_diffrn_reflns_theta_min         1.068
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6605
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0721 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.8859. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       needle
_exptl_crystal_F_000             15648
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.677
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 7820 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(4)
_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     876
_refine_ls_number_reflns         21072
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                18521
_reflns_number_total             21072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00042_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
Adding full bibliography for 4086434--4086438.cif.

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C93 H96 N14 Na2 O7 W2'
_cod_original_formula_weight         1935.51
_cod_original_formula_moiety      'C78 H74 N12 Na2 O6 W2, C5 H12 O, 2(C5 H5 N)'
_cod_original_formula_units_Z            16
_cod_database_code               4086438
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C37
 1.4 with sigma of 0.02
 C37-C38
 1.4 with sigma of 0.02
 C38-C39
 1.4 with sigma of 0.02
 C83-C80
 1.5 with sigma of 0.01
 C81-C80
 1.5 with sigma of 0.02
 H81A-H79C
 1.9 with sigma of 0.04
 H47-H46
 1.92 with sigma of 0.01
 H7-H8
 1.92 with sigma of 0.01
 H10C-C96
 3 with sigma of 0.04
 H10B-C96
 3 with sigma of 0.04
3. Rigid bond restraints
 C78, N11, C74, Na2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N12, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C64, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C70, C71, C72
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.05 and sigma for terminal atoms of 0.05
: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(N11) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uiso(C84) = Uiso(C85) = Uiso(C86) = Uiso(C87) = Uiso(C88)
Uanis(N6) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C39)
Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(N11) = Uanis(C74) = Uanis(C78)
Uiso(C97) = Uiso(C98) = Uiso(N15) = Uiso(C94) = Uiso(C95) = Uiso(C96)
5. Others
 Fixed Sof: C93(0.7) H93(0.7) C92(0.7) H92(0.7) C91(0.7) H91(0.7) C90(0.7)
 H90(0.7) C89(0.7) H89(0.7) N14(0.7) C96(0.3) H96(0.3) C97(0.3) H97(0.3)
 C98(0.3) H98(0.3) N15(0.3) C94(0.3) H94(0.3) C95(0.3) H95(0.3)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C47(H47)
6.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C46(H46), C45(H45), C44(H44), C60(H60), C4(H4), C16(H16),
 C3(H3), C29(H29), C56(H56), C15(H15), C7(H7), C30(H30), C6(H6), C57(H57),
 C5(H5), C12(H12), C39(H39), C38(H38), C37(H37), C36(H36), C35(H35), C58(H58),
 C51(H51), C59(H59), C21(H21), C64(H64), C68(H68), C17(H17), C66(H66), C32(H32),
  C52(H52), C13(H13), C54(H54), C55(H55), C14(H14), C25(H25), C65(H65),
 C53(H53), C33(H33), C28(H28), C69(H69), C34(H34), C73(H73), C67(H67), C31(H31),
  C26(H26), C18(H18), C19(H19), C27(H27), C20(H20), C70(H70), C71(H71),
 C72(H72), C78(H78), C77(H77), C76(H76), C75(H75), C74(H74), C85(H85), C86(H86),
  C87(H87), C88(H88), C84(H84), C93(H93), C92(H92), C91(H91), C90(H90),
 C89(H89), C96(H96), C97(H97), C98(H98), C94(H94), C95(H95)
6.c Fitted hexagon refined as free rotating group:
 N6(C39,C38,C37,C36,C35), N11(C78,C77,C76,C75,C74), C85(C86,C87,C88,N13,C84),
 C93(C92,C91,C90,C89,N14), C96(C97,C98,N15,C94,C95)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C49(H49A,H49B,H49C), C48(H48A,H48B,
 H48C), C79(H79A,H79B,H79C), C82(H82A,H82B,H82C), C81(H81A,H81B,H81C), C83(H83A,
 H83B,H83C)
;
_shelx_res_checksum              92163
_shelx_hkl_checksum              73235
_olex2_submission_special_instructions 'No special instructions were received'