#------------------------------------------------------------------------------
#$Date: 2020-08-06 17:00:18 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254978 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/47/7704707.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704707
loop_
_publ_author_name
'Zhou, Xueer'
'Vasko, Petra'
'Hicks, Jamie'
'Fuentes, M Ángeles'
'Heilmann, Andreas'
'Kolychev, Eugene L.'
'Aldridge, Simon'
_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         'C31 H33 Cl Ge N P'
_chemical_formula_sum            'C31 H33 Cl Ge N P'
_chemical_formula_weight         558.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                111.357(3)
_cell_angle_beta                 92.618(3)
_cell_angle_gamma                90.475(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1837(3)
_cell_length_b                   11.0396(4)
_cell_length_c                   14.5439(5)
_cell_measurement_reflns_used    7455
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.4670
_cell_measurement_theta_min      3.2610
_cell_volume                     1371.34(9)
_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_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11314
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.460
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83079
_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_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0250
_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/[σ²(Fo²)+(0.0330P)²+0.5624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5273
_reflns_number_total             5691
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01960g2.cif
_cod_data_source_block           307xzjh19_a
_cod_depositor_comments
'Adding full bibliography for 7704706--7704714.cif.'
_cod_database_code               7704707
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.886
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.62067(2) 0.55600(2) 0.66662(2) 0.02152(6) Uani 1 1 d . . . . .
Cl1 Cl 0.87024(4) 0.55041(4) 0.64225(3) 0.03296(9) Uani 1 1 d . . . . .
P1 P 0.59972(4) 0.31741(3) 0.58442(2) 0.01803(8) Uani 1 1 d . . . . .
N1 N 0.62450(13) 0.52097(12) 0.78454(8) 0.0192(2) Uani 1 1 d . . . . .
C1 C 0.56501(16) 0.62551(14) 0.86500(10) 0.0206(3) Uani 1 1 d . . . . .
C2 C 0.41913(16) 0.61285(15) 0.88862(11) 0.0230(3) Uani 1 1 d . . . . .
C3 C 0.36121(18) 0.71478(17) 0.96531(12) 0.0299(3) Uani 1 1 d . . . . .
H3 H 0.263601 0.707282 0.981992 0.036 Uiso 1 1 calc R U . . .
C4 C 0.44301(19) 0.82686(17) 1.01777(12) 0.0333(4) Uani 1 1 d . . . . .
H4 H 0.401515 0.895164 1.069839 0.040 Uiso 1 1 calc R U . . .
C5 C 0.58458(19) 0.83893(16) 0.99419(12) 0.0309(3) Uani 1 1 d . . . . .
H5 H 0.639797 0.916181 1.030294 0.037 Uiso 1 1 calc R U . . .
C6 C 0.64862(17) 0.73989(14) 0.91826(11) 0.0242(3) Uani 1 1 d . . . . .
C7 C 0.80586(17) 0.75923(15) 0.89688(12) 0.0274(3) Uani 1 1 d . . . . .
H7 H 0.834148 0.678969 0.841806 0.033 Uiso 1 1 calc R U . . .
C8 C 0.8243(2) 0.8743(2) 0.8632(2) 0.0489(5) Uani 1 1 d . . . . .
H8A H 0.757989 0.862057 0.805585 0.073 Uiso 1 1 calc R U . . .
H8B H 0.925124 0.879494 0.845402 0.073 Uiso 1 1 calc R U . . .
H8C H 0.801430 0.954950 0.917020 0.073 Uiso 1 1 calc R U . . .
C9 C 0.9081(2) 0.7757(2) 0.98726(15) 0.0442(5) Uani 1 1 d . . . . .
H9A H 0.881860 0.853251 1.042777 0.066 Uiso 1 1 calc R U . . .
H9B H 1.009021 0.785578 0.971351 0.066 Uiso 1 1 calc R U . . .
H9C H 0.898785 0.698887 1.005404 0.066 Uiso 1 1 calc R U . . .
C10 C 0.32818(16) 0.48958(16) 0.83401(11) 0.0262(3) Uani 1 1 d . . . . .
H10 H 0.351635 0.459233 0.762809 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3721(2) 0.38187(19) 0.87285(14) 0.0417(4) Uani 1 1 d . . . . .
H11A H 0.359169 0.412076 0.944134 0.063 Uiso 1 1 calc R U . . .
H11B H 0.474554 0.361121 0.860081 0.063 Uiso 1 1 calc R U . . .
H11C H 0.310611 0.303882 0.839035 0.063 Uiso 1 1 calc R U . . .
C12 C 0.1643(2) 0.5083(2) 0.83891(17) 0.0493(5) Uani 1 1 d . . . . .
H12A H 0.136470 0.530250 0.907231 0.074 Uiso 1 1 calc R U . . .
H12B H 0.113180 0.427689 0.796403 0.074 Uiso 1 1 calc R U . . .
H12C H 0.137796 0.578989 0.816237 0.074 Uiso 1 1 calc R U . . .
C13 C 0.73576(17) 0.44802(15) 0.81549(11) 0.0255(3) Uani 1 1 d . . . . .
H13A H 0.713754 0.451643 0.882435 0.031 Uiso 1 1 calc R U . . .
H13B H 0.830373 0.494739 0.821824 0.031 Uiso 1 1 calc R U . . .
C14 C 0.75657(15) 0.30643(14) 0.75195(10) 0.0194(3) Uani 1 1 d . . . . .
C15 C 0.84343(16) 0.23857(15) 0.79797(11) 0.0246(3) Uani 1 1 d . . . . .
H15 H 0.881684 0.283053 0.863674 0.029 Uiso 1 1 calc R U . . .
C16 C 0.87502(18) 0.10893(16) 0.75056(13) 0.0293(3) Uani 1 1 d . . . . .
H16 H 0.933858 0.065657 0.783800 0.035 Uiso 1 1 calc R U . . .
C17 C 0.82067(18) 0.04202(15) 0.65431(13) 0.0299(3) Uani 1 1 d . . . . .
H17 H 0.840490 -0.047413 0.621725 0.036 Uiso 1 1 calc R U . . .
C18 C 0.73743(16) 0.10728(14) 0.60666(12) 0.0249(3) Uani 1 1 d . . . . .
H18 H 0.701581 0.062256 0.540444 0.030 Uiso 1 1 calc R U . . .
C19 C 0.70470(14) 0.23902(14) 0.65419(10) 0.0191(3) Uani 1 1 d . . . . .
C20 C 0.64295(16) 0.24128(14) 0.45532(10) 0.0222(3) Uani 1 1 d . . . . .
C21 C 0.7688(2) 0.2819(2) 0.42380(13) 0.0426(5) Uani 1 1 d . . . . .
H21 H 0.833583 0.344374 0.470215 0.051 Uiso 1 1 calc R U . . .
C22 C 0.7998(3) 0.2313(3) 0.32457(16) 0.0635(8) Uani 1 1 d . . . . .
H22 H 0.885819 0.259358 0.303382 0.076 Uiso 1 1 calc R U . . .
C23 C 0.7066(3) 0.1406(2) 0.25662(14) 0.0517(6) Uani 1 1 d . . . . .
H23 H 0.728401 0.106117 0.188852 0.062 Uiso 1 1 calc R U . . .
C24 C 0.5814(2) 0.09991(18) 0.28732(12) 0.0361(4) Uani 1 1 d . . . . .
H24 H 0.517115 0.037380 0.240543 0.043 Uiso 1 1 calc R U . . .
C25 C 0.54920(17) 0.14996(15) 0.38612(11) 0.0268(3) Uani 1 1 d . . . . .
H25 H 0.462717 0.121819 0.406717 0.032 Uiso 1 1 calc R U . . .
C26 C 0.41026(15) 0.27437(14) 0.58764(10) 0.0212(3) Uani 1 1 d . . . . .
C27 C 0.30631(17) 0.34026(17) 0.55212(12) 0.0279(3) Uani 1 1 d . . . . .
H27 H 0.336693 0.403113 0.525981 0.034 Uiso 1 1 calc R U . . .
C28 C 0.15916(18) 0.31446(19) 0.55480(13) 0.0346(4) Uani 1 1 d . . . . .
H28 H 0.088751 0.359476 0.530488 0.042 Uiso 1 1 calc R U . . .
C29 C 0.11451(18) 0.22266(19) 0.59309(14) 0.0363(4) Uani 1 1 d . . . . .
H29 H 0.013478 0.205161 0.595045 0.044 Uiso 1 1 calc R U . . .
C30 C 0.21681(18) 0.15651(17) 0.62843(13) 0.0330(3) Uani 1 1 d . . . . .
H30 H 0.185736 0.093494 0.654212 0.040 Uiso 1 1 calc R U . . .
C31 C 0.36523(17) 0.18227(15) 0.62623(12) 0.0260(3) Uani 1 1 d . . . . .
H31 H 0.435375 0.137377 0.650860 0.031 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Cl1 98.96(4) . . ?
N1 Ge1 P1 84.39(4) . . ?
Cl1 Ge1 P1 90.494(14) . . ?
C26 P1 C19 107.05(7) . . ?
C26 P1 C20 104.98(7) . . ?
C19 P1 C20 107.73(7) . . ?
C26 P1 Ge1 106.09(5) . . ?
C19 P1 Ge1 110.45(5) . . ?
C20 P1 Ge1 119.75(5) . . ?
C1 N1 C13 114.19(11) . . ?
C1 N1 Ge1 112.05(9) . . ?
C13 N1 Ge1 125.68(10) . . ?
C6 C1 C2 120.18(13) . . ?
C6 C1 N1 121.17(13) . . ?
C2 C1 N1 118.64(13) . . ?
C3 C2 C1 118.53(14) . . ?
C3 C2 C10 120.29(14) . . ?
C1 C2 C10 121.16(13) . . ?
C4 C3 C2 121.41(15) . . ?
C5 C4 C3 119.83(15) . . ?
C4 C5 C6 121.34(15) . . ?
C5 C6 C1 118.71(14) . . ?
C5 C6 C7 118.53(14) . . ?
C1 C6 C7 122.75(13) . . ?
C6 C7 C8 111.93(14) . . ?
C6 C7 C9 110.78(14) . . ?
C8 C7 C9 110.69(16) . . ?
C2 C10 C12 114.14(14) . . ?
C2 C10 C11 109.99(13) . . ?
C12 C10 C11 110.02(16) . . ?
N1 C13 C14 119.09(12) . . ?
C19 C14 C15 117.62(13) . . ?
C19 C14 C13 128.15(13) . . ?
C15 C14 C13 114.19(13) . . ?
C16 C15 C14 122.03(14) . . ?
C15 C16 C17 119.99(14) . . ?
C18 C17 C16 119.11(15) . . ?
C17 C18 C19 121.32(14) . . ?
C14 C19 C18 119.89(13) . . ?
C14 C19 P1 122.02(11) . . ?
C18 C19 P1 118.07(11) . . ?
C21 C20 C25 119.08(14) . . ?
C21 C20 P1 118.87(12) . . ?
C25 C20 P1 121.91(11) . . ?
C22 C21 C20 120.09(17) . . ?
C23 C22 C21 120.42(18) . . ?
C22 C23 C24 119.82(17) . . ?
C23 C24 C25 120.26(16) . . ?
C24 C25 C20 120.33(15) . . ?
C27 C26 C31 119.70(14) . . ?
C27 C26 P1 117.31(11) . . ?
C31 C26 P1 122.96(11) . . ?
C28 C27 C26 120.31(15) . . ?
C27 C28 C29 119.93(16) . . ?
C30 C29 C28 120.25(15) . . ?
C29 C30 C31 120.13(16) . . ?
C30 C31 C26 119.68(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.8894(12) . ?
Ge1 Cl1 2.3330(4) . ?
Ge1 P1 2.4659(4) . ?
P1 C26 1.8071(14) . ?
P1 C19 1.8089(14) . ?
P1 C20 1.8203(15) . ?
N1 C1 1.4440(17) . ?
N1 C13 1.4598(17) . ?
C1 C6 1.415(2) . ?
C1 C2 1.416(2) . ?
C2 C3 1.394(2) . ?
C2 C10 1.521(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.377(2) . ?
C5 C6 1.397(2) . ?
C6 C7 1.520(2) . ?
C7 C8 1.529(2) . ?
C7 C9 1.534(2) . ?
C10 C12 1.522(2) . ?
C10 C11 1.540(2) . ?
C13 C14 1.5175(19) . ?
C14 C19 1.4014(19) . ?
C14 C15 1.404(2) . ?
C15 C16 1.384(2) . ?
C16 C17 1.390(2) . ?
C17 C18 1.381(2) . ?
C18 C19 1.406(2) . ?
C20 C21 1.392(2) . ?
C20 C25 1.392(2) . ?
C21 C22 1.389(3) . ?
C22 C23 1.378(3) . ?
C23 C24 1.381(3) . ?
C24 C25 1.386(2) . ?
C26 C27 1.396(2) . ?
C26 C31 1.396(2) . ?
C27 C28 1.384(2) . ?
C28 C29 1.389(3) . ?
C29 C30 1.386(3) . ?
C30 C31 1.394(2) . ?
