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_7709582
_publ_section_title
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 Assembly of metallo-macrocycles through reductive C--C coupling of
 alkylnitriles by an Mg--Mg-bonded compound
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00181K
_journal_year                    2022
_chemical_formula_moiety         'C132 H207 K3 Mg3 N12 O6'
_chemical_formula_sum            'C132 H207 K3 Mg3 N12 O6'
_chemical_formula_weight         2248.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
_cell_angle_beta                 94.340(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.600(15)
_cell_length_b                   21.925(11)
_cell_length_c                   22.450(11)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    196(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.28
_cell_volume                     14528(13)
_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      195.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0603
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.314
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1291 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.9015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         24405
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1582P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2141
_refine_ls_wR_factor_ref         0.2373
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                17059
_reflns_number_total             24405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00181k3.cif
_cod_data_source_block           1_a_sq
_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        14527(12)
_cod_database_code               7709582
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(6)
 0.03(6)
2. 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
3. Restrained distances
 C114-C115
 1.54 with sigma of 0.02
 C15-C14
 1.54 with sigma of 0.02
4. Rigid bond restraints
 C114, C115
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C117) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) = Uanis(C76)
Uanis(C15) = Uanis(C16)
Uanis(C117) = Uanis(C118)
6.a Ternary CH refined with riding coordinates:
 C43(H43), C46(H46), C55(H55), C58(H58), C67(H67), C70(H70), C79(H79),
 C82(H82), C91(H91), C94(H94), C103(H103), C106(H106)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C22(H22A,H22B), C23(H23A,
 H23B), C26(H26A,H26B), C30(H30A,H30B), C31(H31A,H31B), C34(H34A,H34B),
 C109(H10M,H10N), C110(H11D,H11E), C111(H11F,H11G), C112(H11H,H11I), C113(H11J,
 H11K), C114(H11L,H11M), C115(H11N,H11O), C116(H11P,H11Q), C117(H11R,H11S),
 C118(H11T,H11U), C119(H11V,H11W), C120(H12D,H12E), C121(H12F,H12G), C122(H12H,
 H12I), C123(H12J,H12K), C124(H12L,H12M), C125(H12N,H12O), C126(H12P,H12Q),
 C127(H12R,H12S), C128(H12T,H12U), C129(H12V,H12W), C130(H13D,H13E), C131(H13F,
 H13G), C132(H13H,H13I)
6.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C40(H40), C41(H41), 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), N7(H7), N9(H9), N11(H11)
6.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), C17(H17A,H17B,H17C),
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), 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)
;
_shelx_res_checksum              95239
_shelx_hkl_checksum              15654
_shelx_fab_checksum              27180
_olex2_submission_special_instructions 'No special instructions were received'