Reductive linear- and cyclo-trimerization of isocyanides using an Al‒Al-bonded compound
Chen, Weixing; Zhao, Yanxia; Xu, Wenhua; Su, Ji-Hu; Shen, Lingyi; Liu, Li; Wu, Biao; Yang, Xiao-Juan; Chemical Communications  (2019) –; doi:10.1039/C9CC04344F

data_7123890
_publ_section_title
;
 Reductive linear- and cyclo-trimerization of isocyanides using an
 Al--Al-bonded compound
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04344F
_journal_year                    2019
_chemical_formula_moiety         'C80 H115 Al2 N8 Na O2'
_chemical_formula_sum            'C84 H131 Al2 N8 Na O3'
_chemical_formula_weight         1377.91
_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   mixed
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.599(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.844(9)
_cell_length_b                   26.227(14)
_cell_length_c                   20.493(13)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.40
_cell_volume                     9090(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.994
_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  0.0822
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112677
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         2.236
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1398 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.6464.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.4817
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         15994
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+4.0781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8520
_reflns_number_total             15994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04344f6.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        9089(9)
_cod_database_code               7123890
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.980
_platon_squeeze_void_probe_radius 1.20
_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. Uiso/Uaniso restraints and constraints
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C71) = Uanis(C71A)
Uanis(C72) = Uanis(C72A)
Uanis(C69) = Uanis(C69A)
Uanis(C70) = Uanis(C70A)
3. Others
 Fixed Sof: C69(0.5) C70(0.5) C71(0.5) C72(0.5) C69A(0.5) C71A(0.5) C72A(0.5)
 C70A(0.5)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26), C39(H39), C42(H42), C51(H51), C54(H54)
4.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C19(H19), C20(H20), C21(H21), C35(H35), C36(H36), C37(H37), C47(H47),
 C48(H48), C49(H49)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C)
;
_shelx_res_checksum              33375
_shelx_fab_checksum              71601
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'