Salt metathesis routes to homoleptic near-linear Mg(ii) and Ca(ii) bulky bis(silyl)amide complexes.
Leng, Ji-Dong; Goodwin, Conrad A. P.; Vitorica-Yrezabal, Iñigo J; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12526–12533; doi:10.1039/c8dt00802g

data_7045999
_publ_section_title
;
 Salt metathesis routes to homoleptic near-linear Mg(ii) and Ca(ii) bulky
 bis(silyl)amide complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12526
_journal_page_last               12533
_journal_paper_doi               10.1039/c8dt00802g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C28 H68 Mg N2 O Si4'
_chemical_formula_sum            'C28 H68 Mg N2 O Si4'
_chemical_formula_weight         585.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                115.021(5)
_cell_angle_beta                 90.373(4)
_cell_angle_gamma                93.593(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0810(5)
_cell_length_b                   14.7993(8)
_cell_length_c                   15.5138(8)
_cell_measurement_reflns_used    5731
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      28.1370
_cell_measurement_theta_min      3.0360
_cell_volume                     2091.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_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      1.00  43.00   1.00   10.00    --   21.65 -57.00   0.00   42
  2  \w     38.00  64.00   1.00   10.00    --   21.65 -99.00  30.00   26
  3  \w      9.00  76.00   1.00   10.00    --   21.65  37.00-120.00   67
  4  \w      2.00  94.00   1.00   10.00    --   21.65  77.00 -30.00   92
  5  \w     -8.00  82.00   1.00   10.00    --   21.65  77.00-120.00   90
  6  \w    -50.00  47.00   1.00   10.00    --   21.65 -77.00 120.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0517311000
_diffrn_orient_matrix_UB_12      -0.0068184000
_diffrn_orient_matrix_UB_13      -0.0338641000
_diffrn_orient_matrix_UB_21      0.0393047000
_diffrn_orient_matrix_UB_22      0.0287187000
_diffrn_orient_matrix_UB_23      -0.0184694000
_diffrn_orient_matrix_UB_31      0.0274950000
_diffrn_orient_matrix_UB_32      -0.0440569000
_diffrn_orient_matrix_UB_33      -0.0325800000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14116
_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         25.350
_diffrn_reflns_theta_min         2.534
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.930
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7652
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0384P)^2^+0.5051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6135
_reflns_number_total             7652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00802g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045998--7046003.cif.'
_cod_database_code               7045999
_manchester_internal_coll_name   adpm232
_manchester_internal_coll_client JDL
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 10s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   JDL
_manchester_internal_coll_date   1/9/15
_manchester_internal_process_user CAPG
_manchester_internal_process_date 15/2/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 16/2/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 17/2/18
_manchester_internal_validation_user IVJY
_manchester_internal_validation_date 23/2/18
_manchester_internal_archive_date 23/2/18
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         MgN2Si4C50H60
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27A-C26A \\sim C27B-C26B
 with sigma of 0.02
 C26A-C25 \\sim C26B-C25 \\sim C28-C27B \\sim C28-C27A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(H25C)=Sof(H25D)=Sof(H28C)=Sof(H28D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=
 Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(H28A)=Sof(H28B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D), C28(H28A,H28B), C28(H28C,H28D), C26A(H26A,
 H26B), C27A(H27A,H27B), C26B(H26C,H26D), C27B(H27C,H27D)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              66918
_shelx_fab_checksum              26915
_olex2_exptl_crystal_mounting_method 'From fomlin on a microscope slide.'
_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 1.196
_oxdiff_exptl_absorpt_empirical_full_min 0.768