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_7042261
_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 H70 Mg2 N2 O2 Si2'
_chemical_formula_sum            'C38 H70 Mg2 N2 O2 Si2'
_chemical_formula_weight         691.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4729(5)
_cell_length_b                   17.2445(6)
_cell_length_c                   32.0382(9)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.38
_cell_measurement_theta_min      4.12
_cell_volume                     7996.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega -110.00  -78.00   1.0000   23.7300
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -30.0000 32

  2 omega  -43.00   21.00   1.0000   23.7300
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000  120.0000 64

  3 omega  -17.00   21.00   1.0000   23.7300
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -150.0000 38

  4 omega  -45.00  -19.00   1.0000   23.7300
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  -30.0000 26

  5 omega  -65.00  -38.00   1.0000   23.7300
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -150.0000 27

  6 omega   31.00  110.00   1.0000   94.9300
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -180.0000 79

  7 omega   53.00   91.00   1.0000   94.9300
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   60.0000 38

  8 omega   57.00  133.00   1.0000   94.9300
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000   30.0000 76

  9 omega   37.00   84.00   1.0000   94.9300
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  150.0000 47

 10 omega   51.00   83.00   1.0000   94.9300
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -30.0000 32
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0515765000
_diffrn_orient_matrix_UB_12      -0.0402789000
_diffrn_orient_matrix_UB_13      0.0360686000
_diffrn_orient_matrix_UB_21      -0.0745941000
_diffrn_orient_matrix_UB_22      -0.0277418000
_diffrn_orient_matrix_UB_23      -0.0307995000
_diffrn_orient_matrix_UB_31      0.0555476000
_diffrn_orient_matrix_UB_32      -0.0748406000
_diffrn_orient_matrix_UB_33      -0.0079199000
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            21583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.635
_diffrn_reflns_theta_min         4.117
_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    1.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+2.1224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7262
_reflns_number_total             7994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_original_cell_volume        7996.0(4)
_cod_database_code               7042261
_nottingham_internal_coll_name   MGMBLW
_nottingham_internal_coll_number 12296
_nottingham_internal_coll_client MB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '23.7300 and 94.9300'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   MB
_nottingham_internal_coll_date   12/4/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 09/05/2013
_nottingham_internal_process_user MB
_nottingham_internal_solution_date 09/05/2013
_nottingham_internal_solution_user MB
_nottingham_internal_refinement_date 18/02/2104
_nottingham_internal_refinement_user MB
_nottingham_internal_self_archive_date 25/2/2014
_nottingham_internal_self_validation_date 18/02/2104
_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         C38H70Mg2N2O2Si2
_chemical_oxdiff_usercomment
'MGMBLW #12296 in fomblin film on micromount for MB/DLK'
_reflns_odcompleteness_completeness 99.91
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C20-C21 \\sim C20-C22 \\sim C20A-C21A \\sim C20A-C22
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C20A, C20, C21, C21A, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=1-FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C17(H17), C20(H20), C20A(H20A), C23(H23), C26(H26)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
5.c Me refined with riding coordinates:
 C22(H22D,H22E,H22F), C22(H22A,H22B,H22C)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C),
 C21A(H21D,H21E,H21F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              94827
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'