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_7042258
_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         'C36 H34 N2 Si2'
_chemical_formula_sum            'C36 H34 N2 Si2'
_chemical_formula_weight         550.83
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-02-07 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                100.086(5)
_cell_angle_beta                 92.916(4)
_cell_angle_gamma                106.819(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8529(5)
_cell_length_b                   12.7192(7)
_cell_length_c                   12.8221(8)
_cell_measurement_reflns_used    4691
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.15
_cell_measurement_theta_min      4.57
_cell_volume                     1505.56(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(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 0.986
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
  1 omega  -73.00   26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1627   77.0000 -180.0000 99

  2 omega  -25.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1627  -57.0000  -90.0000 93

  3 omega   18.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1627   57.0000   60.0000 94

  4 omega   43.00   70.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -125.0000   30.0000 27

  5 omega   67.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   15.0000  120.0000 91

  6 omega   38.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000   60.0000 34

  7 omega   34.00   69.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -30.0000  -30.0000 35

  8 omega   46.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -77.0000   30.0000 86

  9 omega   35.00   69.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -30.0000 -150.0000 34

 10 omega   59.00  115.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -125.0000 -150.0000 56

 11 omega   68.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   15.0000    0.0000 90

 12 omega   67.00  157.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   15.0000 -120.0000 90

 13 omega   34.00   69.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -30.0000   90.0000 35

 14 omega   48.00  137.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -77.0000  -90.0000 89

 15 omega   90.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -125.0000   30.0000 31

 16 omega   73.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000 -150.0000 35

 17 omega   57.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -61.0000  150.0000 67
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type
'SuperNova, single source at offset (Cu), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0069353000
_diffrn_orient_matrix_UB_12      -0.0269526000
_diffrn_orient_matrix_UB_13      -0.1224246000
_diffrn_orient_matrix_UB_21      -0.0138650000
_diffrn_orient_matrix_UB_22      0.1167436000
_diffrn_orient_matrix_UB_23      -0.0044848000
_diffrn_orient_matrix_UB_31      0.1635669000
_diffrn_orient_matrix_UB_32      0.0480894000
_diffrn_orient_matrix_UB_33      0.0077136000
_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_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9878
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.017
_diffrn_reflns_theta_min         3.522
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.332
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.4706
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.0853
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5860
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0715P)^2^+0.7771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5168
_reflns_number_total             5860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           L2H2
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_original_cell_volume        1505.55(15)
_cod_database_code               7042258
_nottingham_internal_coll_name   MGMBLU
_nottingham_internal_coll_number 12166
_nottingham_internal_coll_client MB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '16.0000 and 4.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   MB
_nottingham_internal_coll_date   1/2/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 05/02/2013
_nottingham_internal_process_user MB
_nottingham_internal_solution_date 05/02/2013
_nottingham_internal_solution_user MB
_nottingham_internal_refinement_date 18/012/2014
_nottingham_internal_refinement_user MB
_nottingham_internal_self_archive_date 21/2/2014
_nottingham_internal_self_validation_date 18/02/2014
_nottingham_internal_self_validation_user MB
_nottingham_internal_validation_date 25/10/2016
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 25/10/2016
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C35 H34 N2 Si2'
_chemical_oxdiff_usercomment
'MGMBLU #12166 IN FOMBLIN FILM ON MICROMOUNT FOR MB/DLK'
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H2 of N2
 At 1.5 times of:
  All C(H,H,H) groups, H1 of N1
2. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), 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)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              78499
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2013-02-01
_olex2_date_sample_submission    2013-01-15
_olex2_submission_special_instructions 'No special instructions were received'