1,8-Bis(silylamido)naphthalene complexes of magnesium and zinc synthesised through alkane elimination reactions.
Bradley, Mark A.; Birchall, Chris; Blake, Alexander J.; Lewis, William; Moxey, Graeme J.; Kays, Deborah L.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4101–4110; doi:10.1039/c7dt00471k

data_7042259
_publ_section_title
;
 1,8-Bis(silylamido)naphthalene complexes of magnesium and zinc
 synthesised through alkane elimination reactions.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4101
_journal_page_last               4110
_journal_paper_doi               10.1039/c7dt00471k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C44 H48 Mg N2 O2 Si2'
_chemical_formula_sum            'C44 H48 Mg N2 O2 Si2'
_chemical_formula_weight         717.33
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2017-02-07 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                75.089(6)
_cell_angle_beta                 80.260(7)
_cell_angle_gamma                72.972(8)
_cell_formula_units_Z            2
_cell_length_a                   8.6851(9)
_cell_length_b                   11.9556(8)
_cell_length_c                   20.1125(13)
_cell_measurement_reflns_used    3825
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.19
_cell_measurement_theta_min      3.96
_cell_volume                     1919.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -98.00   -5.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  125.0000  -90.0000 93

  2 omega -115.00  -29.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  -38.0000   60.0000 86

  3 omega -112.00  -14.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  -77.0000 -180.0000 98

  4 omega   41.00   72.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   60.0000 31

  5 omega   35.00  131.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000   30.0000 96

  6 omega   54.00  139.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -157.0000 -106.0000 85

  7 omega   39.00   77.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -180.0000 38

  8 omega   39.00   77.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   90.0000 38

  9 omega  126.00  154.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000   90.0000 28

 10 omega   35.00  134.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000  -90.0000 99

 11 omega   38.00   77.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -90.0000 39

 12 omega   35.00   63.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -119.0000   46.0000 28

 13 omega   82.00  118.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -119.0000   46.0000 36

 14 omega   83.00  125.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000   90.0000 42

 15 omega   66.00  158.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   15.0000  -30.0000 92

 16 omega   42.00  142.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472    0.0000   90.0000 100

 17 omega   27.00  110.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -137.0000 83
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1845980000
_diffrn_orient_matrix_UB_12      0.0303052000
_diffrn_orient_matrix_UB_13      -0.0015239000
_diffrn_orient_matrix_UB_21      -0.0240542000
_diffrn_orient_matrix_UB_22      -0.0128971000
_diffrn_orient_matrix_UB_23      0.0790145000
_diffrn_orient_matrix_UB_31      -0.0108808000
_diffrn_orient_matrix_UB_32      0.1341814000
_diffrn_orient_matrix_UB_33      -0.0101503000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1263
_diffrn_reflns_av_unetI/netI     0.1497
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12398
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.965
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  1.015
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.0898
_exptl_crystal_size_min          0.0256
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6694
_refine_ls_number_restraints     777
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.1128
_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^)+(0.0301P)^2^+19.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2528
_refine_ls_wR_factor_ref         0.2775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4053
_reflns_number_total             6694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_database_code               7042259
_nottingham_internal_coll_name   MGMBLA
_nottingham_internal_coll_number 10226
_nottingham_internal_coll_client MB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '50 and 200'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   10/5/2011
_nottingham_internal_process_date 13/05/2011
_nottingham_internal_process_user WL
_nottingham_internal_solution_user MB
_nottingham_internal_refinement_date 26/1/2015
_nottingham_internal_refinement_user MB/WL
_nottingham_internal_self_archive_date 26/01/2015
_nottingham_internal_self_validation_date 26/01/2015
_nottingham_internal_self_validation_user pczwl
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44 H48 Mg N2 O2 Si2'
_chemical_oxdiff_usercomment
'MGMBLA #10226 IN FOMBLIN FILM ON MICORMOUNT FOR MB/DLK'
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.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), C43(H43A,H43B), C44(H44A,H44B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              10348
_olex2_submission_special_instructions 'No special instructions were received'