Unsupported metal silyl ether coordination.
Pahl, Jürgen; Elsen, Holger; Friedrich, Alexander; Harder, Sjoerd; Chemical communications (Cambridge, England) 54 (2018) 7846–7849; doi:10.1039/c8cc04517h

data_7121854
_publ_section_title
;
 Unsupported metal silyl ether coordination.
;
_journal_issue                   56
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7846
_journal_page_last               7849
_journal_paper_doi               10.1039/c8cc04517h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C35 H59 Mg N2 O Si2, C6 H5 Cl, B C24 F20'
_chemical_formula_sum            'C65 H64 B Cl F20 Mg N2 O Si2'
_chemical_formula_weight         1395.93
_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             2017-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                98.233(4)
_cell_angle_beta                 97.872(4)
_cell_angle_gamma                90.686(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3518(6)
_cell_length_b                   14.4685(7)
_cell_length_c                   17.3377(7)
_cell_measurement_reflns_used    11623
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6150
_cell_measurement_theta_min      3.7020
_cell_volume                     3281.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -55.00  33.00   1.00    1.00    --  -41.15  38.00-120.00   88
  2  \w    -74.00  32.00   1.00    1.00    --  -41.15  77.00 -30.00  106
  3  \w    -82.00   5.00   1.00    1.00    --  -41.15  19.00-180.00   87
  4  \w     23.00  96.00   1.00    1.00    --   41.15-125.00 120.00   73
  5  \w     34.00 129.00   1.00    3.00    --  106.54 -45.00  30.00   95
  6  \w     95.00 178.00   1.00    3.00    --  106.54  45.00 120.00   83
  7  \w     94.00 178.00   1.00    3.00    --  106.54 125.00 -60.00   84
  8  \w     91.00 178.00   1.00    3.00    --  106.54  45.00  60.00   87
  9  \w     83.00 178.00   1.00    3.00    --  106.54  77.00   0.00   95
 10  \w     58.00 109.00   1.00    3.00    --  106.54 -94.00  30.00   51
 11  \w     39.00 122.00   1.00    3.00    --  106.54-125.00 -60.00   83
 12  \w     34.00 134.00   1.00    3.00    --  106.54 -61.00 -90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0760753000
_diffrn_orient_matrix_UB_12      -0.0775305000
_diffrn_orient_matrix_UB_13      -0.0431090000
_diffrn_orient_matrix_UB_21      -0.0532604000
_diffrn_orient_matrix_UB_22      0.0046306000
_diffrn_orient_matrix_UB_23      0.0738028000
_diffrn_orient_matrix_UB_31      -0.0704096000
_diffrn_orient_matrix_UB_32      0.0745268000
_diffrn_orient_matrix_UB_33      -0.0302815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20747
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.594
_diffrn_reflns_theta_min         3.088
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0507P)^2^+0.9270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11206
_reflns_number_total             12606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04517h2.cif
_cod_data_source_block           hasj170608a
_cod_depositor_comments          'Adding full bibliography for 7121854.cif.'
_cod_original_cell_volume        3281.9(3)
_cod_database_code               7121854
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F O Si'
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C12(H12), C27(H27), C24(H24), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C22(H22), C10(H10), C20(H20), C21(H21), C64(H64),
 C65(H65), C60(H60), C61(H61), C62(H62)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C),
 C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C31(H31A,
 H31B,H31C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_olex2_date_sample_data_collection 2017-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.829