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_7042265
_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         'C80 H84 I2 Mg2 N4 O2 Si4, C4 H10 O'
_chemical_formula_sum            'C84 H94 I2 Mg2 N4 O3 Si4'
_chemical_formula_weight         1622.41
_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             2015-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-02-07 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                69.427(3)
_cell_angle_beta                 75.353(4)
_cell_angle_gamma                85.388(4)
_cell_formula_units_Z            1
_cell_length_a                   10.827(2)
_cell_length_b                   13.846(3)
_cell_length_c                   14.987(3)
_cell_measurement_reflns_used    2267
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.35
_cell_volume                     2035.0(7)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      90(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.1147
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17889
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0765 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8299.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.524
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0838
_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^)+(0.0202P)^2^+1.2799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6208
_reflns_number_total             9167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00471k1.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7042258--7042265.cif.'
_cod_database_code               7042265
_nottingham_internal_coll_name   MGMBLF
_nottingham_internal_coll_number 10987
_nottingham_internal_coll_client MB/DLK
_nottingham_internal_solution_user mb
_nottingham_internal_refinement_date 18/7/2015
_nottingham_internal_refinement_user pczwl/MB
_nottingham_internal_validation_date 18/7/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 18/7/2015
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 Si1-C18 \\sim Si1-C18A
 with sigma of 0.02
 C19A-C18A \\sim C19-C18 \\sim C23A-C18A \\sim C23-C18
 with sigma of 0.02
 Si1-C18 \\sim Si1-C18A
 with sigma of 0.02
 C20-C19 \\sim C20A-C19A \\sim C23A-C22A \\sim C23-C22
 with sigma of 0.02
 C18-C20 \\sim C18-C22 \\sim C18A-C20A \\sim C18A-C22A
 with sigma of 0.02
 C19-C23 \\sim C19A-C23A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.02
 C22A-C21A \\sim C22-C21 \\sim C21A-C20A \\sim C21-C20
 with sigma of 0.02
 C19-C21 \\sim C23-C21 \\sim C19A-C21A \\sim C21A-C23A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20 \\sim C20A \\sim C21
\\sim C21A \\sim C22 \\sim C22A \\sim C23 \\sim C23A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
O2 \\sim C41 \\sim C41 \\sim C43 \\sim C44: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Si1, C18, C18A, C19, C19A, C20, C20A, C21, C21A, C22, C22A, C23, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C41, H41A, H41B, C42, H42A, H42B, H42C, C43, H43A, H43B, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23)=1-FVAR(1)
 Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=FVAR(1)
 Fixed Sof: O2(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
6.a Ternary CH refined with riding coordinates:
 C6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C19A(H19A), C20(H20), C20A(H20A), C21(H21),
 C21A(H21A), C22(H22), C22A(H22A), C23(H23), C23A(H23A), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              27367
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'