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_7042264
_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 H52 I2 Mg2 N2 O2 Si2'
_chemical_formula_sum            'C44 H52 I2 Mg2 N2 O2 Si2'
_chemical_formula_weight         999.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-24
_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                90
_cell_angle_beta                 93.943(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2536(7)
_cell_length_b                   10.1900(3)
_cell_length_c                   21.7038(7)
_cell_measurement_reflns_used    14629
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.58
_cell_measurement_theta_min      4.08
_cell_volume                     4468.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      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 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -77.00   20.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877   19.0000 -180.0000 97

  2 omega  -25.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  -38.0000  -90.0000 86

  3 omega   53.00   94.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  162.0000  125.0000 41

  4 omega  102.00  154.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   61.0000 -180.0000 52

  5 omega   27.00  102.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  -90.0000 75

  6 omega  102.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000   60.0000 56

  7 omega   33.00   65.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   60.0000 32

  8 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  125.0000  120.0000 85

  9 omega   41.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   30.0000 27

 10 omega   36.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   90.0000 33

 11 omega   39.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   90.0000 33

 12 omega   47.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -30.0000 26

 13 omega   89.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   15.0000  -30.0000 68

 14 omega   81.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  -60.0000 26

 15 omega   43.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -90.0000 26

 16 omega -112.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -57.0000 -180.0000 93

 17 omega -115.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -77.0000  -60.0000 101

 18 omega -112.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -57.0000   30.0000 93

 19 omega -116.00  -48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877 -162.0000   98.0000 68

 20 omega   80.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   61.0000  150.0000 78

 21 omega   33.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -162.0000  -81.0000 110

 22 omega   85.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000  120.0000 73

 23 omega   36.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -120.0000 41

 24 omega   33.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000    0.0000 36

 25 omega   27.00  110.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000   60.0000 83

 26 omega   85.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000    0.0000 73

 27 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -120.0000 75

 28 omega -112.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -57.0000   90.0000 93

 29 omega -112.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -57.0000  -30.0000 93

 30 omega -115.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -77.0000 -180.0000 101

 31 omega    2.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877 -125.0000   60.0000 96

 32 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   72.0000  -86.0000 81

 33 omega   80.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   61.0000   60.0000 78

 34 omega   80.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   61.0000   30.0000 78
;
_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      0.0436289000
_diffrn_orient_matrix_UB_12      -0.1074214000
_diffrn_orient_matrix_UB_13      -0.0261644000
_diffrn_orient_matrix_UB_21      -0.0140655000
_diffrn_orient_matrix_UB_22      0.0565194000
_diffrn_orient_matrix_UB_23      -0.0654510000
_diffrn_orient_matrix_UB_31      0.0608690000
_diffrn_orient_matrix_UB_32      0.0902391000
_diffrn_orient_matrix_UB_33      0.0098189000
_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  0.0735
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.758
_diffrn_reflns_theta_min         4.083
_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    12.129
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.5096
_exptl_crystal_size_mid          0.3941
_exptl_crystal_size_min          0.3736
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0966P)^2^+19.4823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4428
_reflns_number_total             4528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_database_code               7042264
_nottingham_internal_coll_name   MGMBLH
_nottingham_internal_coll_number 11094
_nottingham_internal_coll_client MB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '2.0000 and 4.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   29/1/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 30/01/2012
_nottingham_internal_process_user WL
_nottingham_internal_solution_date 30/1/2012
_nottingham_internal_solution_user MB
_nottingham_internal_refinement_date 30/1/2012
_nottingham_internal_refinement_user MB
_nottingham_internal_validation_date 24/10/2016
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 24/10/2016
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C44 H52 I2 Mg2 N2 O2 Si2'
_chemical_oxdiff_usercomment
'MGMBLH #11094 IN FOMBLIN FILM ON MICROMOUNT FOR MB/DLK'
_reflns_odcompleteness_completeness 99.88
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              43592
_olex2_date_sample_data_collection 2012-01-29
_olex2_date_sample_submission    2012-01-10
_olex2_submission_special_instructions 'No special instructions were received'