Assembly of metallo-macrocycles through reductive C–C coupling of alkylnitriles by an Mg–Mg-bonded compound
Xue, Yujie; Wang, Jijiang; Shi, Yalei; Xu, Wenhua; Zhao, Yanxia; Wu, Biao; Yang, Xiao-Juan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00181K

data_7709583
_publ_section_title
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 Assembly of metallo-macrocycles through reductive C--C coupling of
 alkylnitriles by an Mg--Mg-bonded compound
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00181K
_journal_year                    2022
_chemical_formula_moiety         'C139.09 H218 K3 Mg3 N12 O7, 0.45(C2)'
_chemical_formula_sum            'C140 H227 K3 Mg3 N12 O7'
_chemical_formula_weight         2380.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                95.42(4)
_cell_angle_beta                 97.06(4)
_cell_angle_gamma                108.92(4)
_cell_formula_units_Z            2
_cell_length_a                   14.10(3)
_cell_length_b                   17.32(3)
_cell_length_c                   34.45(6)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.38
_cell_volume                     7817(3)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.980
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            91362
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.509
_diffrn_reflns_theta_min         2.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1374 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.8786.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.011
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0038(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1500
_refine_ls_number_reflns         28510
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.1148
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+26.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2297
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14110
_reflns_number_total             28510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00181k3.cif
_cod_data_source_block           1_a_sq_CCDC1
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        7817(25)
_cod_database_code               7709583
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C20
 1.54 with sigma of 0.02
 C20-C21 = C21-C22 = C128-C129
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C19A)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128)
\\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(C42) = Uanis(C47)
Uanis(C20) = Uanis(C21)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C130) = Uanis(C131)
Uanis(C22) = Uanis(C23)
Uanis(C25) = Uanis(C26)
Uanis(C26) = Uanis(C27)
4. Others
 Sof(C19A)=Sof(C20A)=Sof(C21A)=1-FVAR(1)
 Sof(C19)=Sof(C20)=Sof(C21)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C55(H55), C67(H67), C70(H70), C79(H79), C82(H82), C91(H91), C94(H94),
 C103(H103), C106(H106), C115(H115), C118(H118), C125(H125)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C41(H41A,H41B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C122(H12J,
 H12K), C123(H12L,H12M), C126(H12Q,H12R), C127(H12S,H12T), C128(H12U,H12V),
 C129(H12W,H12X), C130(H13D,H13E), C131(H13F,H13G), C132(H13H,H13I), C133(H13J,
 H13K), C134(H13L,H13M), C135(H13N,H13O), C136(H13P,H13Q), C137(H13R,H13S),
 C139(H13W,H13X), C140(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N9(H9), N11(H11), C51(H51), C52(H52), C53(H53), C63(H63), C64(H64),
 C65(H65), C75(H75), C76(H76), C77(H77), C87(H87), C88(H88), C89(H89), C99(H99),
  C100(H100), C101(H101), C111(H111), C112(H112), C113(H113)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C),
 C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C),
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,
 H96B,H96C), C104(H10A,H10B,H10C), C105(H10D,H10E,H10F), C107(H10G,H10H,H10I),
 C108(H10J,H10K,H10L), C116(H11D,H11E,H11F), C117(H11G,H11H,H11I), C119(H11J,
 H11K,H11L), C120(H12D,H12E,H12F), C121(H12G,H12H,H12I), C124(H12N,H12O,H12P),
 C138(H13T,H13U,H13V), C141(H14E,H14F,H14G)
;
_shelx_res_checksum              60762
_shelx_hkl_checksum              60552
_shelx_fab_checksum              85008
_olex2_submission_special_instructions 'No special instructions were received'