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_7045998
_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         'C48 H54 K N O3 Si2'
_chemical_formula_sum            'C48 H54 K N O3 Si2'
_chemical_formula_weight         788.20
_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
_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                70.553(5)
_cell_angle_beta                 75.294(6)
_cell_angle_gamma                62.990(7)
_cell_formula_units_Z            2
_cell_length_a                   11.7633(8)
_cell_length_b                   12.7083(7)
_cell_length_c                   17.4748(11)
_cell_measurement_reflns_used    3721
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      27.0140
_cell_measurement_theta_min      2.4530
_cell_volume                     2178.2(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      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -11.00  89.00   1.00    5.50    --   18.70  77.00  30.00  100
  2  \w     -8.00  89.00   1.00    5.50    --   18.70  77.00 -90.00   97
  3  \w    -10.00  89.00   1.00    5.50    --   18.70  77.00 150.00   99
;
_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      0.0517042000
_diffrn_orient_matrix_UB_12      0.0169408000
_diffrn_orient_matrix_UB_13      -0.0050462000
_diffrn_orient_matrix_UB_21      -0.0433895000
_diffrn_orient_matrix_UB_22      0.0623519000
_diffrn_orient_matrix_UB_23      -0.0071734000
_diffrn_orient_matrix_UB_31      -0.0096936000
_diffrn_orient_matrix_UB_32      -0.0041547000
_diffrn_orient_matrix_UB_33      0.0424746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11877
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.859
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.478
_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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7938
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+1.6542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             7938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00802g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045998--7046003.cif.'
_cod_database_code               7045998
_manchester_internal_coll_name   adpm271
_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   7/11/15
_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         KNSi2C30H30
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O3-C48B \\sim O3-C48A \\sim O3-C45B \\sim O3-C45A \\sim O2-C44A \\sim O2-C44B
\\sim O2-C41 \\sim O1-C37 ~
 O1-C40
 with sigma of 0.01
 C38-C37 \\sim C39-C40 \\sim C47B-C48B \\sim C48A-C47A \\sim C46B-C45B \\sim
C45A-C46A \\sim C41-C42 ~
 C43A-C44A \\sim C44B-C43B
 with sigma of 0.01
 C43A-C42 \\sim C43B-C42 \\sim C39-C38 \\sim C46B-C47B \\sim C46A-C47A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C42 \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A \\sim C48A \\sim
C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B \\sim C48B: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.004
Uanis(C45B) \\sim Ueq, Uanis(C48B) \\sim Ueq, Uanis(C47B) \\sim Ueq,
Uanis(C46B) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C48A) \\sim Ueq,
Uanis(C47A) \\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=
 Sof(H44D)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=
 Sof(H44B)=FVAR(1)
 Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(C47B)=
 Sof(H47A)=Sof(H47B)=Sof(C48B)=Sof(H48A)=Sof(H48B)=1-FVAR(2)
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C42(H42C,H42D), C43A(H43A,H43B), C44A(H44A,H44B),
 C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D), C48A(H48C,H48D), C43B(H43C,
 H43D), C44B(H44C,H44D), C45B(H45A,H45B), C46B(H46A,H46B), C47B(H47A,H47B),
 C48B(H48A,H48B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              35531
_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.782