Activation of cyclopentadiene derivatives by an α-diimine-ligated Mg-Mg-bonded compound.
Qu, Yao; Xi, Zhixian; Sun, Zhenzhou; Yang, Li; Liu, Rui; Dong, Ben; Wu, Biao; Yang, Xiao-Juan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10065–10069; doi:10.1039/d4dt01038h

data_7716306
_publ_section_title
;
 Activation of cyclopentadiene derivatives by an &#x3b1;-diimine-ligated
 Mg-Mg-bonded compound.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10065
_journal_page_last               10069
_journal_paper_doi               10.1039/d4dt01038h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C100 H148 K4 Mg2 N8 O3'
_chemical_formula_sum            'C100 H148 K4 Mg2 N8 O3'
_chemical_formula_weight         1715.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-26 deposited with the CCDC.	2024-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.445(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8718(8)
_cell_length_b                   24.4841(10)
_cell_length_c                   24.6090(7)
_cell_measurement_reflns_used    15514
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0260
_cell_measurement_theta_min      2.1460
_cell_volume                     11144.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  28.00   0.50   13.00    --    3.55 -99.00 -90.00   80
  2  \w     -8.00  76.00   0.50   13.00    --    3.55  57.00 -90.00  168
  3  \w     13.00  58.00   0.50   13.00    --    3.55  57.00   0.00   90
  4  \w     13.00  51.00   0.50   13.00    --    3.55  19.00  60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.344
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_description       block
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         10959
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1028P)^2^+12.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8389
_reflns_number_total             10959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01038h2.cif
_cod_data_source_block           qy-20230621-1_auto
_cod_depositor_comments
'Adding full bibliography for 7716304--7716306.cif.'
_cod_database_code               7716306
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.979
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O2-C63 = O2-C33
 1.37 with sigma of 0.02
 C63-C57 = C65-C33
 1.32 with sigma of 0.02
 C57-C65
 1.42 with sigma of 0.02
 O2'-C67 = O2'-C35
 1.37 with sigma of 0.02
 C67-C17 = C69-C35
 1.32 with sigma of 0.02
 C17-C69
 1.42 with sigma of 0.02
 H4C-H39B
 2.15 with sigma of 0.02
 H39B-H4B
 2.15 with sigma of 0.02
 O2-C57 = O2-C65 = C63-C65 = C57-C33
 2.21 with sigma of 0.04
 O2'-C17 = O2'-C69 = C67-C69 = C17-C35
 2.21 with sigma of 0.04
 N1-C7
 with sigma of 0.02
 C7-C49
 with sigma of 0.02
 C7-C47
 with sigma of 0.02
 C49-C25
 with sigma of 0.02
 C25-C45
 with sigma of 0.02
 C45-C23
 with sigma of 0.02
 C23-C47
 with sigma of 0.02
 N1-C49
 with sigma of 0.04
 N1-C47
 with sigma of 0.04
 C7-C25
 with sigma of 0.04
 C7-C23
 with sigma of 0.04
 C49-C45
 with sigma of 0.04
 C49-C47
 with sigma of 0.04
 C25-C23
 with sigma of 0.04
 C45-C47
 with sigma of 0.04
 O2-C63 \\sim O2-C33
 with sigma of 0.02
 C63-C57 \\sim C65-C33
 with sigma of 0.02
 O2-C65 \\sim O2-C57
 with sigma of 0.04
 C63-C65 \\sim C57-C33
 with sigma of 0.04
 O2'-C67 \\sim O2'-C35
 with sigma of 0.02
 C67-C17 \\sim C69-C35
 with sigma of 0.02
 O2'-C69 \\sim O2'-C17
 with sigma of 0.04
 C67-C69 \\sim C17-C35
 with sigma of 0.04
3. Restrained planarity
 O2, C63, C57, C65, C33
 with sigma of 0.1
 O2', C67, C17, C69, C35
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.02A with sigma of 3.8 and sigma
for terminal atoms of 0.01 within 0.02A
O2 \\sim C63 \\sim C57 \\sim C65 \\sim C33: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O2' \\sim C67 \\sim C17 \\sim C69 \\sim C35: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O2, C63, C57, C65, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2', C67, C17, C69, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C45)=Sof(H45)=Sof(C23)=Sof(H23)=Sof(C47)=Sof(C7)=Sof(C49)=Sof(C25)=
 Sof(H25)=1-FVAR(1)
 Sof(C52)=Sof(H52)=Sof(C54)=Sof(H54)=Sof(C56)=Sof(C58)=Sof(C60)=Sof(C62)=
 Sof(H62)=FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
 Sof(C72)=Sof(C9)=1-FVAR(3)
 Sof(C2)=Sof(C1)=FVAR(3)
 Sof(C64)=Sof(H64)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=1-FVAR(4)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C61)=Sof(H61)=FVAR(4)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(5)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=FVAR(5)
 Fixed Sof: H37B(0.5) H37A(0.5) H37C(0.5) H37E(0.5) H37D(0.5) H37F(0.5)
 C5(0.5) H5(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C43(0.5) H43(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C51(0.5) H51(0.5) C13(0.5) H13(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 O2(0.4) C63(0.4) H63A(0.4) H63B(0.4) C57(0.4) H57A(0.4) H57B(0.4) C65(0.4)
 H65A(0.4) H65B(0.4) C33(0.4) H33A(0.4) H33B(0.4) O2'(0.6) C67(0.6) H67A(0.6)
 H67B(0.6) C17(0.6) H17A(0.6) H17B(0.6) C69(0.6) H69A(0.6) H69B(0.6) C35(0.6)
 H35A(0.6) H35B(0.6)
7.a Ternary CH refined with riding coordinates:
 C29(H29), C10(H10)
7.b Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C57(H57A,H57B), C65(H65A,H65B), C33(H33A,H33B), C67(H67A,
 H67B), C17(H17A,H17B), C69(H69A,H69B), C35(H35A,H35B)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C24(H24), C26(H26), C28(H28), C30(H30), C32(H32), C34(H34),
 C38(H38), C40(H40), C44(H44), C45(H45), C23(H23), C25(H25)
7.d Fitted hexagon refined as free rotating group:
 C45(C23,C47,C7,C49,C25)
7.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C46(H46A,H46B,H46C), C48(H48A,H48B,
 H48C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39127
_shelx_fab_checksum              76269
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;