Cationic aza-macrocyclic complexes of germanium(ii) and silicon(iv).
Everett, Matthew; Jolleys, Andrew; Levason, William; Light, Mark E.; Pugh, David; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20898–20905; doi:10.1039/c5dt03941j

data_7037200
_publ_section_title
;
 Cationic aza-macrocyclic complexes of germanium(ii) and silicon(iv).
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20898
_journal_page_last               20905
_journal_paper_doi               10.1039/c5dt03941j
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H28 Ge N4, 2(C F3 O3 S), 0.8(C2 H3 N)'
_chemical_formula_sum            'C15.6 H30.4 F6 Ge N4.8 O6 S2'
_chemical_formula_weight         631.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           103
_space_group_name_Hall           'P 4 -2c'
_space_group_name_H-M_alt        'P 4 c c'
_symmetry_space_group_name_Hall  'P 4 -2c'
_symmetry_space_group_name_H-M   'P 4 c c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.16 svn.r3215 for OlexSys, GUI svn.r5097)
;
_audit_update_record
;
2015-10-07 deposited with the CCDC.
2015-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   17.1253(3)
_cell_length_b                   17.1253(3)
_cell_length_c                   22.1160(10)
_cell_measurement_reflns_used    11249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.2
_cell_volume                     6486.1(3)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 246
               Slice: -110.0000 - 13.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 225.0000
                 XTD: 45.0283
              2theta: -20.0280
scan:
    Number of images: 162
               Slice: -51.0000 - 30.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 45.0000
                 XTD: 45.0283
              2theta: -20.0280
scan:
    Number of images: 52
               Slice: -70.0000 - -44.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -45.0000
                 Phi: 45.0000
                 XTD: 45.0283
              2theta: -20.0280
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.008003
_diffrn_orient_matrix_UB_12      0.056465
_diffrn_orient_matrix_UB_13      -0.011999
_diffrn_orient_matrix_UB_21      0.057722
_diffrn_orient_matrix_UB_22      -0.007690
_diffrn_orient_matrix_UB_23      0.002309
_diffrn_orient_matrix_UB_31      0.000506
_diffrn_orient_matrix_UB_32      -0.009443
_diffrn_orient_matrix_UB_33      -0.044099
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34358
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.695
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       Block
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1901 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7099
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      5.297
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+5.7986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.650
_reflns_Friedel_fraction_full    0.721
_reflns_Friedel_fraction_max     0.684
_reflns_number_gt                5647
_reflns_number_total             7099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03941j2.cif
_cod_data_source_block           2014aj006r_ml
_cod_depositor_comments
'Adding full bibliography for 7037199--7037205.cif.'
_cod_original_cell_volume        6486.1(4)
_cod_original_formula_sum        'C15.60 H30.40 F6 Ge N4.80 O6 S2'
_cod_database_code               7037200
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O12-O11
 2.3 with sigma of 0.02
 O11-O10
 2.3 with sigma of 0.02
 O10-O12
 2.3 with sigma of 0.02
 F12-F11
 2.1 with sigma of 0.02
 F11-F10
 2.1 with sigma of 0.02
 F10-F12
 2.1 with sigma of 0.02
 F6-O10 = O10-F10
 2.9 with sigma of 0.02
 O11-F11
 2.9 with sigma of 0.02
 O12-F12
 2.9 with sigma of 0.02
 C21-O12 = C21-O10 = C21-O11
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S4 \\sim S2 \\sim S1 \\sim S3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O10 \\sim O11 \\sim O12 \\sim O4 \\sim O5 \\sim O6 \\sim O1 \\sim O2 \\sim O3
\\sim O7 \\sim O8 \\sim O9: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F10 \\sim F11 \\sim F12 \\sim F4 \\sim F5 \\sim F6 \\sim F1 \\sim F2 \\sim F3
\\sim F7 \\sim F8 \\sim F9: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C21 \\sim C19 \\sim C18 \\sim C20: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(S1) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{S4, F12, F11, F10, O12, O11, O10, C21} sigma for 1-2: 0.002, 1-3: 0.04
as
{S2, F4, F5, F6, O4, O5, O6, C19}
{S3, F7, F8, F9, O7, O8, O9, C20} sigma for 1-2: 0.02, 1-3: 0.04
as
{S1, F1, F2, F3, O1, O2, O3, C18}
6. Others
 Fixed Sof: S4(0.25) F12(0.25) F11(0.25) F10(0.25) O12(0.25) O11(0.25)
 O10(0.25) C21(0.25) S3(0.25) F7(0.25) F8(0.25) F9(0.25) O7(0.25) O8(0.25)
 O9(0.25) C20(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B), C15(H15A,H15B)
7.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              14680
_shelx_hkl_checksum              64416
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'