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_7716305
_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         'C41 H61 K Mg N2 O'
_chemical_formula_sum            'C41 H61 K Mg N2 O'
_chemical_formula_weight         661.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2816(8)
_cell_length_b                   8.9404(3)
_cell_length_c                   19.5450(6)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.8700
_cell_measurement_theta_min      2.3080
_cell_volume                     3893.5(2)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_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    -78.00   6.00   0.50    3.00    --   -6.75 -57.00  30.00  168
  2  \w    -71.00  -6.00   0.50    3.00    --   -6.75  -8.00 -89.00  130
  3  \w     -3.00  36.00   0.50    3.00    --    3.39 -99.00-120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0313268000
_diffrn_orient_matrix_UB_12      0.0086707000
_diffrn_orient_matrix_UB_13      0.0052587000
_diffrn_orient_matrix_UB_21      -0.0046057000
_diffrn_orient_matrix_UB_22      -0.0001164000
_diffrn_orient_matrix_UB_23      0.0358888000
_diffrn_orient_matrix_UB_31      0.0034272000
_diffrn_orient_matrix_UB_32      -0.0788542000
_diffrn_orient_matrix_UB_33      0.0004816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22362
_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         26.014
_diffrn_reflns_theta_min         2.278
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93006
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.5824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6226
_reflns_number_total             7055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01038h2.cif
_cod_data_source_block           qy-20230526_auto
_cod_depositor_comments
'Adding full bibliography for 7716304--7716306.cif.'
_cod_database_code               7716305
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 O1 K1 Mg1'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.935
_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. Restrained distances
 O1'-C38' = O1'-C41'
 1.44 with sigma of 0.02
 C38'-C39' = C40'-C41'
 1.53 with sigma of 0.02
 C39'-C40'
 1.54 with sigma of 0.02
 O1-C41 = O1-C38
 1.44 with sigma of 0.02
 C41-C40 = C39-C38
 1.53 with sigma of 0.02
 C40-C39
 1.54 with sigma of 0.02
 O1'-C39' = O1'-C40' = C38'-C40' = C39'-C41'
 2.38 with sigma of 0.04
 O1-C40 = O1-C39 = C41-C39 = C40-C38
 2.38 with sigma of 0.04
 C38'-C39' \\sim C39'-C40' \\sim C40'-C41'
 with sigma of 0.02
 O1'-C38' \\sim O1'-C41'
 with sigma of 0.02
 O1'-C39' \\sim O1'-C40'
 with sigma of 0.04
 C39'-C41' \\sim C38'-C40'
 with sigma of 0.04
 C41-C40 \\sim C40-C39 \\sim C39-C38
 with sigma of 0.02
 O1-C41 \\sim O1-C38
 with sigma of 0.02
 O1-C40 \\sim O1-C39
 with sigma of 0.04
 C40-C38 \\sim C41-C39
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1' \\sim C38' \\sim C39' \\sim C40' \\sim C41': within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1 \\sim C41 \\sim C40 \\sim C39 \\sim C38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O1', C38', C39', C40', C41'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C41, C40, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1'(0.5) C38'(0.5) H38A(0.5) H38B(0.5) C39'(0.5) H39A(0.5)
 H39B(0.5) C40'(0.5) H40A(0.5) H40B(0.5) C41'(0.5) H41A(0.5) H41B(0.5) O1(0.5)
 C41(0.5) H41C(0.5) H41D(0.5) C40(0.5) H40C(0.5) H40D(0.5) C39(0.5) H39C(0.5)
 H39D(0.5) C38(0.5) H38C(0.5) H38D(0.5)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C23(H23), C11(H11), C26(H26)
6.b Secondary CH2 refined with riding coordinates:
 C38'(H38A,H38B), C39'(H39A,H39B), C40'(H40A,H40B), C41'(H41A,H41B), C41(H41C,
 H41D), C40(H40C,H40D), C39(H39C,H39D), C38(H38C,H38D)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C21(H21), C19(H19), C20(H20), C9(H9), C7(H7), C8(H8)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C35(H35A,H35B,H35C), C24(H24A,H24B,H24C),
 C36(H36A,H36B,H36C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C16(H16A,H16B,
 H16C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C13(H13A,
 H13B,H13C), C27(H27A,H27B,H27C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              90035
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.881