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_7046001
_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         'C20 H46 I Mg N O2 Si2'
_chemical_formula_sum            'C20 H46 I Mg N O2 Si2'
_chemical_formula_weight         539.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3956(6)
_cell_length_b                   7.8668(2)
_cell_length_c                   36.2303(14)
_cell_measurement_reflns_used    5718
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.0370
_cell_measurement_theta_min      2.8440
_cell_volume                     5528.1(3)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -19.00  26.00   0.50   20.00    --  -22.97 -99.00   0.00   90
  2  \w    -69.00  29.00   0.50   20.00    --  -22.97  19.00-180.00  196
  3  \w     37.00 102.00   0.50   20.00    --   23.91 178.00 -60.00  130
;
_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      -0.0310868000
_diffrn_orient_matrix_UB_12      0.0285008000
_diffrn_orient_matrix_UB_13      -0.0082769000
_diffrn_orient_matrix_UB_21      0.0188409000
_diffrn_orient_matrix_UB_22      0.0291326000
_diffrn_orient_matrix_UB_23      -0.0155265000
_diffrn_orient_matrix_UB_31      -0.0041586000
_diffrn_orient_matrix_UB_32      -0.0804070000
_diffrn_orient_matrix_UB_33      -0.0085708000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16211
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.382
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_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    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             5051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00802g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7045998--7046003.cif.'
_cod_database_code               7046001
_manchester_internal_coll_name   adpm261
_manchester_internal_coll_client JDL
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 20s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   JDL
_manchester_internal_coll_date   18/10/15
_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         MgC20N2Si3H30
_reflns_odcompleteness_completeness 99.34
_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
 C15-C14 \\sim C19B-C18 \\sim C19A-C18
 with sigma of 0.01
 C16-C15 \\sim C14-C13 \\sim C18-C17 \\sim C20-C19B \\sim C20-C19A
 with sigma of 0.01
 O1-C16 \\sim O1-C13 \\sim O2-C17 \\sim O2-C20
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim C17 \\sim C18 \\sim C20 \\sim C19A \\sim C19B: within 2A with sigma of
0.008 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H18C)=Sof(H18D)=Sof(H20C)=Sof(H20D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(H20A)=Sof(H20B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C18(H18C,H18D), C20(H20A,H20B), C20(H20C,H20D),
 C19A(H19A,H19B), C19B(H19C,H19D)
6.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)
;
_shelx_res_checksum              23685
_olex2_exptl_crystal_mounting_method 'From fomblin 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 2.948
_oxdiff_exptl_absorpt_empirical_full_min 0.439