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_7042262
_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         'C38 H38 N2 Si2 Zn2'
_chemical_formula_sum            'C38 H38 N2 Si2 Zn2'
_chemical_formula_weight         709.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
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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                90
_cell_angle_beta                 96.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9259(3)
_cell_length_b                   16.7724(4)
_cell_length_c                   20.3979(5)
_cell_measurement_reflns_used    6367
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.4132
_cell_measurement_theta_min      3.4186
_cell_volume                     3371.70(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega  -27.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -77.0000  150.0000 95

  2 omega  -20.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9127  -38.0000 -180.0000 85

  3 omega   45.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  150.0000 26

  4 omega   91.00  149.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -120.0000 58

  5 omega   36.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -123.0000  -38.0000 77

  6 omega  107.00  157.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  120.0000 50

  7 omega   48.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -129.0000 -127.0000 50

  8 omega   88.00  158.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -180.0000 70

  9 omega  107.00  154.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  125.0000 -150.0000 47

 10 omega   30.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -103.0000   55.0000 77
;
_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      0.0146636000
_diffrn_orient_matrix_UB_12      -0.0914865000
_diffrn_orient_matrix_UB_13      0.0012629000
_diffrn_orient_matrix_UB_21      0.0253196000
_diffrn_orient_matrix_UB_22      0.0019325000
_diffrn_orient_matrix_UB_23      0.0760177000
_diffrn_orient_matrix_UB_31      -0.1534382000
_diffrn_orient_matrix_UB_32      -0.0083766000
_diffrn_orient_matrix_UB_33      0.0033510000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13642
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.584
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    2.646
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
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    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.1407
_exptl_crystal_size_mid          0.0993
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0551P)^2^+1.6255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             6643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_database_code               7042262
_nottingham_internal_coll_name   ZNCBLB
_nottingham_internal_coll_number 10048
_nottingham_internal_coll_client CB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '10 and 40'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_user   wl
_nottingham_internal_coll_date   3/3/2011
_nottingham_internal_process_date 03/03/2011
_nottingham_internal_process_user wl
_nottingham_internal_solution_date 11/07/2013
_nottingham_internal_solution_user CB
_nottingham_internal_refinement_date 26/01/2015
_nottingham_internal_refinement_user CB/wl
_nottingham_internal_self_archive_date 26/01/2015
_nottingham_internal_self_validation_date 26/01/2015
_nottingham_internal_self_validation_user WL
_nottingham_internal_validation_date 25/10/2016
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 25/10/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C38 H38 N2 Si2 Zn2'
_chemical_oxdiff_usercomment
'ZNCBLB #10048 IN FOMBLIN FILM ON MICROMOUNT FOR CB/DLK'
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              61020
_olex2_submission_special_instructions 'No special instructions were received'