Cooperative N-H bond activation by amido-Ge(ii) cations.
Zhou, Xueer; Vasko, Petra; Hicks, Jamie; Fuentes, M Ángeles; Heilmann, Andreas; Kolychev, Eugene L.; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9495–9504; doi:10.1039/d0dt01960g

data_7704713
_publ_section_title
;
 Cooperative N-H bond activation by amido-Ge(ii) cations.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9495
_journal_page_last               9504
_journal_paper_doi               10.1039/d0dt01960g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H42 Ge N2 P, Al C16 F36 O4'
_chemical_formula_sum            'C59 H42 Al F36 Ge N2 O4 P'
_chemical_formula_weight         1657.48
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.236(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.6853(7)
_cell_length_b                   18.4131(3)
_cell_length_c                   29.1049(8)
_cell_measurement_reflns_used    8817
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      74.9490
_cell_measurement_theta_min      3.8500
_cell_volume                     13281.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -15.00  28.00   1.00   25.00    --  -42.66  38.00 -30.00   43
  2  \w    -22.00  21.00   1.00   25.00    --  -42.66  38.00 -60.00   43
  3  \w    -44.00  -4.00   1.00   25.00    --  -42.66  38.00-150.00   40
  4  \w    -10.00  27.00   1.00   25.00    --  -42.66  38.00  30.00   37
  5  \w     85.00 126.00   1.00   25.00    --   42.66 178.00  30.00   41
  6  \w     68.00 116.00   1.00   25.00    --   42.66 178.00-120.00   48
  7  \w     62.00  88.00   1.00   90.00    --  111.00 -95.00 150.00   26
  8  \w     88.00 119.00   1.00   90.00    --  111.00  45.00 -60.00   31
  9  \w     40.00  96.00   1.00   90.00    --  111.00 -45.00-180.00   56
 10  \w    140.00 166.00   1.00   90.00    --  111.00  15.00 -90.00   26
 11  \w    112.00 138.00   1.00   90.00    --  111.00 -61.00-180.00   26
 12  \w    126.00 175.00   1.00   90.00    --  111.00  45.00 -60.00   49
 13  \w     48.00  79.00   1.00   90.00    --  111.00 -30.00 -60.00   31
 14  \w     58.00  85.00   1.00   90.00    --  111.00 -61.00-180.00   27
 15  \w    128.00 154.00   1.00   90.00    --  111.00  30.00   0.00   26
 16  \w     88.00 116.00   1.00   90.00    --  111.00  30.00   0.00   28
 17  \w     69.00  95.00   1.00   90.00    --  111.00 -45.00 120.00   26
 18  \w    111.00 177.00   1.00   90.00    --  111.00 125.00 150.00   66
 19  \w     37.00  90.00   1.00   90.00    --  111.00 -30.00  30.00   53
 20  \w     67.00 107.00   1.00   90.00    --  111.00  15.00 -90.00   40
 21  \w     42.00  78.00   1.00   90.00    --  111.00-125.00-180.00   36
 22  \w     41.00  99.00   1.00   90.00    --  111.00 -77.00 150.00   58
 23  \w     38.00  82.00   1.00   90.00    --  111.00 -30.00 120.00   44
 24  \w     66.00 107.00   1.00   90.00    --  111.00  15.00 120.00   41
 25  \w     -6.00  -5.00   1.00   25.00    --  -42.66  38.00-150.00    1
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0055357000
_diffrn_orient_matrix_UB_12      -0.0742770000
_diffrn_orient_matrix_UB_13      0.0266887000
_diffrn_orient_matrix_UB_21      -0.0616667000
_diffrn_orient_matrix_UB_22      -0.0029597000
_diffrn_orient_matrix_UB_23      -0.0239602000
_diffrn_orient_matrix_UB_31      -0.0058724000
_diffrn_orient_matrix_UB_32      -0.0384204000
_diffrn_orient_matrix_UB_33      -0.0496135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38546
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.164
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             6608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         13689
_refine_ls_number_restraints     1001
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1044P)^2^+35.1211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10222
_reflns_number_total             13689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01960g2.cif
_cod_data_source_block           069xzah19
_cod_depositor_comments
'Adding full bibliography for 7704706--7704714.cif.'
_cod_original_cell_volume        13281.4(7)
_cod_database_code               7704713
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H50P1N1Ge1Al1O4F40
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.799
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 F8A-C47A = F9A-C47A = F7A-C47A = F3A-C45A = F2A-C45A = F1A-C45A = F6A-C46A =
 F4A-C46A = F5A-C46A
 1.33 with sigma of 0.008
 C59A-C56A = C57A-C56A = C58A-C56A
 1.53 with sigma of 0.008
 F36A-C59A = F34A-C59A = F35A-C59A = F28A-C57A = F30A-C57A = F29A-C57A = F31A-
 C58A = F33A-C58A = F32A-C58A
 1.33 with sigma of 0.008
 C45-F1 = C45-F2 = C45-F3
 1.33 with sigma of 0.008
 C47-C44 = C47A-C44 = C45-C44 = C45A-C44 = C46-C44 = C46A-C44
 1.53 with sigma of 0.008
 F8-C47 = F9-C47 = F7-C47 = F6-C46 = F4-C46 = F5-C46 = F1-C45 = F2-C45 = F3-C45
 1.33 with sigma of 0.008
 C58-C56 = C59-C56 = C57-C56
 1.53 with sigma of 0.008
 F36-C59 = F34-C59 = F35-C59 = F32-C58 = F33-C58 = F31-C58 = F30-C57 = F29-C57
 = F28-C57
 1.33 with sigma of 0.008
 O4-C56A = O4-C56
 1.33 with sigma of 0.008
 C53-C52 = C55-C52 = C54-C52
 1.53 with sigma of 0.008
 C55A-C52A = C54A-C52A = C53A-C52A
 1.53 with sigma of 0.008
 F26-C55 = F26A-C55A = F25A-C55A = F25-C55 = F27A-C55A = F27-C55 = F21-C53 =
 F19-C53 = F19A-C53A = F20A-C53A = F21A-C53A = F22A-C54A = F22-C54 = F23A-C54A =
  F23-C54 = F24A-C54A = F24-C54
 1.33 with sigma of 0.008
 F26A-F25A
 2.13 with sigma of 0.008
 F25A-F27A
 2.13 with sigma of 0.008
 F27A-F26A
 2.13 with sigma of 0.008
 F21A-F19A
 2.13 with sigma of 0.008
 F6A-F5A
 2.13 with sigma of 0.008
 F5A-F4A
 2.13 with sigma of 0.008
 F4A-F6A
 2.13 with sigma of 0.008
 F1A-F3A
 2.13 with sigma of 0.008
 F3A-F2A
 2.13 with sigma of 0.008
 F2A-F1A
 2.13 with sigma of 0.008
 F9A-F7A
 2.13 with sigma of 0.008
 F7A-F8A
 2.13 with sigma of 0.008
 F8A-F9A
 2.13 with sigma of 0.008
 C47A-C45A
 2.5 with sigma of 0.008
 C45A-C46A
 2.5 with sigma of 0.008
 C46A-C47A
 2.5 with sigma of 0.008
 C59A-C57A
 2.5 with sigma of 0.008
 C57A-C58A
 2.5 with sigma of 0.008
 C58A-C59A
 2.5 with sigma of 0.008
 F7-F8
 2.13 with sigma of 0.008
 F8-F9
 2.13 with sigma of 0.008
 F9-F7
 2.13 with sigma of 0.008
 F6-F4
 2.13 with sigma of 0.008
 F6-F5
 2.13 with sigma of 0.008
 F5-F4
 2.13 with sigma of 0.008
 C47-C45
 2.5 with sigma of 0.008
 C47-C46
 2.5 with sigma of 0.008
 C46-C45
 2.5 with sigma of 0.008
 C57-C59
 2.5 with sigma of 0.008
 C58-C59
 2.5 with sigma of 0.008
 C58-C57
 2.5 with sigma of 0.008
 F36-F35
 2.13 with sigma of 0.008
 F36-F34
 2.13 with sigma of 0.008
 F35-F34
 2.13 with sigma of 0.008
 F32A-F31A
 2.13 with sigma of 0.008
 F31A-F33A
 2.13 with sigma of 0.008
 F33A-F32A
 2.13 with sigma of 0.008
 F35A-F34A
 2.13 with sigma of 0.008
 F34A-F36A
 2.13 with sigma of 0.008
 F36A-F35A
 2.13 with sigma of 0.008
 F29A-F28A
 2.13 with sigma of 0.008
 F28A-F30A
 2.13 with sigma of 0.008
 F30A-F29A
 2.13 with sigma of 0.008
 F23A-F22A
 2.13 with sigma of 0.008
 F20A-F21A
 2.13 with sigma of 0.008
 F19A-F20A
 2.13 with sigma of 0.008
 C54A-C53A = C53A-C55A = C55A-C54A
 2.5 with sigma of 0.008
 C54-C53 = C53-C55 = C55-C54
 2.5 with sigma of 0.008
 F22A-F24A
 2.13 with sigma of 0.008
 F24A-F23A
 2.13 with sigma of 0.008
 F23A-F24A
 2.13 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
F9A \\sim F7A \\sim F8A \\sim F3A \\sim F2A \\sim F1A \\sim F5A \\sim F6A \\sim
F4A: within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
F21 \\sim F19 \\sim F20 \\sim F24 \\sim F22 \\sim F23 \\sim F26 \\sim F25 \\sim
F27: within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
F8 \\sim F9 \\sim F7 \\sim F3 \\sim F2 \\sim F1 \\sim F5 \\sim F6 \\sim F4:
within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
C45 \\sim C45A \\sim C46 \\sim C46A \\sim C47 \\sim C47A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C47 \\sim C47A \\sim C45 \\sim C45A \\sim C44 \\sim C46 \\sim C46A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
C58A \\sim C56A \\sim C59A \\sim C57A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
F31A \\sim C58A \\sim F33A \\sim F32A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
F30A \\sim C57A \\sim F29A \\sim F28A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C59A \\sim F36A \\sim F35A \\sim F34A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C54 \\sim C52 \\sim C53 \\sim C55: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C53A \\sim C52A \\sim C55A \\sim C54A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C55A \\sim F26A \\sim F27A \\sim F25A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C54A \\sim F23A \\sim F22A \\sim F24A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C53A \\sim F21A \\sim F20A \\sim F19A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Sof(F26A)=Sof(F25A)=Sof(F20A)=Sof(F27A)=Sof(F21A)=Sof(F19A)=Sof(F24A)=
 Sof(F22A)=Sof(F23A)=Sof(C55A)=Sof(C54A)=Sof(C53A)=Sof(C52A)=1-FVAR(1)
 Sof(F26)=Sof(F25)=Sof(C52)=Sof(F20)=Sof(F27)=Sof(F21)=Sof(F19)=Sof(F24)=
 Sof(F22)=Sof(F23)=Sof(C55)=Sof(C54)=Sof(C53)=FVAR(1)
 Sof(F7A)=Sof(F9A)=Sof(F8A)=Sof(C46A)=Sof(F5A)=Sof(F1A)=Sof(F6A)=Sof(C47A)=
 Sof(C45A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(F7)=Sof(F9)=Sof(F8)=Sof(C46)=Sof(F5)=Sof(F1)=Sof(F6)=Sof(C47)=Sof(C45)=
 Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(F35A)=Sof(F36A)=Sof(F31A)=Sof(F34A)=Sof(F33A)=Sof(F32A)=Sof(C59A)=
 Sof(C56A)=Sof(F28A)=Sof(F29A)=Sof(F30A)=Sof(C57A)=Sof(C58A)=1-FVAR(3)
 Sof(F35)=Sof(F36)=Sof(F31)=Sof(F34)=Sof(F33)=Sof(F32)=Sof(C59)=Sof(C56)=
 Sof(F28)=Sof(F29)=Sof(F30)=Sof(C57)=Sof(C58)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C33(H33), C42(H42), C2(H2), C34(H34), C19(H19), C18(H18), C16(H16),
 C11(H11), C17(H17), C36(H36), C39(H39), C22(H22), C10(H10), C5(H5), C9(H9),
 C4(H4), C13(H13), C3(H3), C41(H41), C12(H12), C35(H35), C40(H40), C23(H23),
 C24(H24)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              24332
_shelx_hkl_checksum              19835
_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 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.874