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_7046000
_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         'C72 H60 Mg N2 Si4'
_chemical_formula_sum            'C72 H60 Mg N2 Si4'
_chemical_formula_weight         1089.89
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9967(4)
_cell_length_b                   13.9967(4)
_cell_length_c                   14.5303(6)
_cell_measurement_reflns_used    8505
_cell_measurement_temperature    100.00(1)
_cell_measurement_theta_max      74.5560
_cell_measurement_theta_min      4.3800
_cell_volume                     2846.60(16)
_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_temperature      100.000(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    102.65 244.65   2.00   20.00    --  112.00  73.87-145.79   71
  2  \w    -98.44  57.56   2.00   15.00    --  -70.00  73.87 -85.79   78
  3  \f    106.63 330.61   2.00   20.00  99.21 113.00  73.87    --   112
  4  \f     59.31 281.29   2.00   20.00 161.47 110.00  73.87    --   111
  5  \w    -31.39  70.61   2.00   15.00    --  -80.00  73.87 174.21   51
  6  \w    -44.29  49.71   2.00   15.00    --  -15.00  73.87 -50.79   47
  7  \f    227.78 311.77   2.00   20.00-135.79 110.00  73.87    --    42
  8  \f      3.70 139.68   2.00   20.00 108.82 110.00  73.87    --    68
  9  \f     32.34 102.27   2.00   15.00 -34.23 -14.50  73.87    --    35
 10  \w    160.80 232.80   2.00   20.00    --  113.00  73.87 174.21   36
 11  \w    124.35 210.35   2.00   20.00    --  100.00  73.87  89.21   43
 12  \w    143.98 213.98   2.00   20.00    --  110.00  73.87  34.21   35
 13  \w    174.71 246.71   2.00   20.00    --   90.00  73.87  -0.79   36
 14  \f    162.43 258.42   2.00   20.00 143.19 110.00  73.87    --    48
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0346747000
_diffrn_orient_matrix_UB_12      0.0634550000
_diffrn_orient_matrix_UB_13      0.0797931000
_diffrn_orient_matrix_UB_21      0.0668909000
_diffrn_orient_matrix_UB_22      0.0535500000
_diffrn_orient_matrix_UB_23      -0.0665186000
_diffrn_orient_matrix_UB_31      -0.0803344000
_diffrn_orient_matrix_UB_32      0.0722642000
_diffrn_orient_matrix_UB_33      -0.0208278000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17572
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.206
_diffrn_reflns_theta_min         4.386
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 1020 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0463P)^2^+0.4933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2450
_reflns_number_total             2604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00802g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7045998--7046003.cif.'
_cod_original_cell_volume        2846.6(2)
_cod_database_code               7046000
_manchester_internal_coll_name   adpm271
_manchester_internal_coll_client JDL
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 15/20s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w and \f scans'
_manchester_internal_coll_user   JDL
_manchester_internal_coll_date   21/12/15
_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         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.763
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a 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)
;
_shelx_res_checksum              95586
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.528
_oxdiff_exptl_absorpt_empirical_full_min 0.735