#------------------------------------------------------------------------------
#$Date: 2019-07-08 10:23:27 +0300 (Mon, 08 Jul 2019) $
#$Revision: 216816 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552007.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_1552007
loop_
_publ_author_name
'Arnab Rit'
'Jesus Campos'
'Haoyu Niu'
'Simon Aldridge'
_publ_section_title
;
 A stable heavier group 14 analogue of vinylidene
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1022
_journal_page_last               1026
_journal_paper_doi               10.1038/nchem.2597
_journal_volume                  8
_journal_year                    2016
_chemical_formula_sum            'C52 H76 B2 Ge2 N4'
_chemical_formula_weight         923.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.648(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6923(3)
_cell_length_b                   12.3401(2)
_cell_length_c                   15.7584(4)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.1356
_cell_measurement_theta_min      3.5788
_cell_volume                     2638.92(10)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    .
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.294
_diffrn_reflns_theta_min         4.021
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_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     287
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0299
_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/[σ²(Fo²)+(0.0502P)²+0.7678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4605
_reflns_number_total             5226
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nchem.2597-s8.cif
_cod_data_source_block           105arjc15_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1552007
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.54117(2) 0.50401(2) 0.57246(2) 0.02917(8) Uani 1 1 d . . . . .
H1B H 0.6179(17) 0.4182(18) 0.5825(14) 0.052(6) Uiso 1 1 d . . . . .
H2B H 0.5998(18) 0.6099(19) 0.5805(15) 0.059(7) Uiso 1 1 d . . . . .
N1 N 0.44915(9) 0.39387(9) 0.72050(7) 0.0246(2) Uani 1 1 d . . . . .
N2 N 0.37111(9) 0.55128(9) 0.68264(7) 0.0252(2) Uani 1 1 d . . . . .
B1 B 0.45002(12) 0.48367(12) 0.66379(10) 0.0226(3) Uani 1 1 d . . . . .
C1 C 0.37243(11) 0.40837(12) 0.76973(9) 0.0299(3) Uani 1 1 d . . . . .
H1 H 0.3557 0.3597 0.8122 0.036 Uiso 1 1 calc R U . . .
C2 C 0.32612(12) 0.50201(11) 0.74743(11) 0.0300(3) Uani 1 1 d . . . . .
H2 H 0.2716 0.5303 0.7717 0.036 Uiso 1 1 calc R U . . .
C3 C 0.51820(10) 0.30729(12) 0.73778(9) 0.0277(3) Uani 1 1 d . . . . .
C4 C 0.51446(12) 0.21948(12) 0.68102(10) 0.0343(3) Uani 1 1 d . . . . .
C5 C 0.58234(17) 0.13600(15) 0.70094(14) 0.0541(5) Uani 1 1 d . . . . .
H5 H 0.5819 0.0755 0.6636 0.065 Uiso 1 1 calc R U . . .
C6 C 0.65006(18) 0.1399(2) 0.77393(16) 0.0661(7) Uani 1 1 d . . . . .
H6 H 0.6948 0.0815 0.7869 0.079 Uiso 1 1 calc R U . . .
C7 C 0.65345(15) 0.2269(2) 0.82780(14) 0.0580(6) Uani 1 1 d . . . . .
H7 H 0.7010 0.2285 0.8775 0.070 Uiso 1 1 calc R U . . .
C8 C 0.58802(12) 0.31381(15) 0.81092(11) 0.0385(4) Uani 1 1 d . . . . .
C9 C 0.43672(14) 0.21497(13) 0.60350(11) 0.0399(4) Uani 1 1 d . . . . .
H9 H 0.4258 0.2906 0.5815 0.048 Uiso 1 1 calc R U . . .
C10 C 0.33974(17) 0.17446(19) 0.62911(15) 0.0573(5) Uani 1 1 d . . . . .
H10A H 0.3487 0.1011 0.6526 0.086 Uiso 1 1 calc R U . . .
H10B H 0.2894 0.1734 0.5787 0.086 Uiso 1 1 calc R U . . .
H10C H 0.3186 0.2229 0.6725 0.086 Uiso 1 1 calc R U . . .
C11 C 0.4654(2) 0.1456(2) 0.53043(15) 0.0695(7) Uani 1 1 d . . . . .
H11A H 0.5290 0.1703 0.5154 0.104 Uiso 1 1 calc R U . . .
H11B H 0.4149 0.1523 0.4804 0.104 Uiso 1 1 calc R U . . .
H11C H 0.4708 0.0696 0.5486 0.104 Uiso 1 1 calc R U . . .
C12 C 0.59622(14) 0.41252(17) 0.86866(11) 0.0478(4) Uani 1 1 d . . . . .
H12 H 0.5411 0.4626 0.8470 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5846(2) 0.3838(3) 0.96061(14) 0.0756(7) Uani 1 1 d . . . . .
H13A H 0.5193 0.3521 0.9625 0.113 Uiso 1 1 calc R U . . .
H13B H 0.5915 0.4495 0.9959 0.113 Uiso 1 1 calc R U . . .
H13C H 0.6355 0.3314 0.9827 0.113 Uiso 1 1 calc R U . . .
C14 C 0.6922(3) 0.4726(3) 0.8638(2) 0.0989(11) Uani 1 1 d . . . . .
H14A H 0.7478 0.4271 0.8876 0.148 Uiso 1 1 calc R U . . .
H14B H 0.6927 0.5401 0.8967 0.148 Uiso 1 1 calc R U . . .
H14C H 0.6979 0.4895 0.8039 0.148 Uiso 1 1 calc R U . . .
C15 C 0.34226(11) 0.65596(11) 0.64829(9) 0.0274(3) Uani 1 1 d . . . . .
C16 C 0.25800(12) 0.66495(13) 0.58793(10) 0.0338(3) Uani 1 1 d . . . . .
C17 C 0.23461(13) 0.76788(14) 0.55350(11) 0.0408(4) Uani 1 1 d . . . . .
H17 H 0.1783 0.7764 0.5118 0.049 Uiso 1 1 calc R U . . .
C18 C 0.29150(14) 0.85645(13) 0.57895(12) 0.0424(4) Uani 1 1 d . . . . .
H18 H 0.2746 0.9254 0.5544 0.051 Uiso 1 1 calc R U . . .
C19 C 0.37323(14) 0.84621(13) 0.64003(11) 0.0391(4) Uani 1 1 d . . . . .
H19 H 0.4113 0.9085 0.6578 0.047 Uiso 1 1 calc R U . . .
C20 C 0.40070(12) 0.74574(12) 0.67598(10) 0.0319(3) Uani 1 1 d . . . . .
C21 C 0.19145(14) 0.56882(15) 0.56296(13) 0.0466(4) Uani 1 1 d . . . . .
H21 H 0.2276 0.5016 0.5841 0.056 Uiso 1 1 calc R U . . .
C22 C 0.09784(18) 0.5759(2) 0.60534(16) 0.0668(6) Uani 1 1 d . . . . .
H22A H 0.1153 0.5785 0.6677 0.100 Uiso 1 1 calc R U . . .
H22B H 0.0567 0.5121 0.5897 0.100 Uiso 1 1 calc R U . . .
H22C H 0.0613 0.6415 0.5859 0.100 Uiso 1 1 calc R U . . .
C23 C 0.16418(16) 0.5587(2) 0.46557(15) 0.0682(7) Uani 1 1 d . . . . .
H23A H 0.1176 0.6162 0.4450 0.102 Uiso 1 1 calc R U . . .
H23B H 0.1337 0.4879 0.4518 0.102 Uiso 1 1 calc R U . . .
H23C H 0.2238 0.5656 0.4378 0.102 Uiso 1 1 calc R U . . .
C24 C 0.48813(14) 0.73530(14) 0.74561(11) 0.0407(4) Uani 1 1 d . . . . .
H24 H 0.5168 0.6615 0.7400 0.049 Uiso 1 1 calc R U . . .
C25 C 0.4539(2) 0.7408(2) 0.83322(13) 0.0692(7) Uani 1 1 d . . . . .
H25A H 0.4247 0.8120 0.8410 0.104 Uiso 1 1 calc R U . . .
H25B H 0.5103 0.7295 0.8776 0.104 Uiso 1 1 calc R U . . .
H25C H 0.4045 0.6842 0.8377 0.104 Uiso 1 1 calc R U . . .
C26 C 0.57016(16) 0.8170(2) 0.73882(14) 0.0579(5) Uani 1 1 d . . . . .
H26A H 0.5881 0.8157 0.6807 0.087 Uiso 1 1 calc R U . . .
H26B H 0.6278 0.7982 0.7799 0.087 Uiso 1 1 calc R U . . .
H26C H 0.5473 0.8898 0.7516 0.087 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'
B B 0.0090 0.0039 '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'
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
B1 Ge1 Ge1 114.21(4) . 3_666
B1 Ge1 H1B 109.1(9) . .
Ge1 Ge1 H1B 107.9(8) 3_666 .
B1 Ge1 H2B 114.2(9) . .
Ge1 Ge1 H2B 106.7(9) 3_666 .
H1B Ge1 H2B 104.1(13) . .
C1 N1 B1 108.56(12) . .
C1 N1 C3 121.13(11) . .
B1 N1 C3 129.85(12) . .
C2 N2 B1 108.46(11) . .
C2 N2 C15 122.70(12) . .
B1 N2 C15 128.71(12) . .
N1 B1 N2 104.74(12) . .
N1 B1 Ge1 126.48(11) . .
N2 B1 Ge1 128.71(10) . .
C2 C1 N1 109.18(13) . .
C2 C1 H1 125.4 . .
N1 C1 H1 125.4 . .
C1 C2 N2 109.06(13) . .
C1 C2 H2 125.5 . .
N2 C2 H2 125.5 . .
C8 C3 C4 122.23(14) . .
C8 C3 N1 118.46(14) . .
C4 C3 N1 119.30(13) . .
C5 C4 C3 117.43(17) . .
C5 C4 C9 122.09(17) . .
C3 C4 C9 120.44(14) . .
C6 C5 C4 121.1(2) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C7 C6 C5 120.62(17) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
C6 C7 C8 121.08(19) . .
C6 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C7 C8 C3 117.56(18) . .
C7 C8 C12 120.47(17) . .
C3 C8 C12 121.93(15) . .
C4 C9 C10 110.07(15) . .
C4 C9 C11 113.95(18) . .
C10 C9 C11 109.69(17) . .
C4 C9 H9 107.6 . .
C10 C9 H9 107.6 . .
C11 C9 H9 107.6 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C14 C12 C8 110.9(2) . .
C14 C12 C13 111.3(2) . .
C8 C12 C13 112.08(19) . .
C14 C12 H12 107.4 . .
C8 C12 H12 107.4 . .
C13 C12 H12 107.4 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 C20 122.28(14) . .
C16 C15 N2 119.25(13) . .
C20 C15 N2 118.47(13) . .
C15 C16 C17 117.42(15) . .
C15 C16 C21 121.84(14) . .
C17 C16 C21 120.69(15) . .
C18 C17 C16 121.18(16) . .
C18 C17 H17 119.4 . .
C16 C17 H17 119.4 . .
C17 C18 C19 120.47(15) . .
C17 C18 H18 119.8 . .
C19 C18 H18 119.8 . .
C18 C19 C20 120.95(16) . .
C18 C19 H19 119.5 . .
C20 C19 H19 119.5 . .
C19 C20 C15 117.67(15) . .
C19 C20 C24 120.90(15) . .
C15 C20 C24 121.37(13) . .
C16 C21 C22 110.68(16) . .
C16 C21 C23 112.38(18) . .
C22 C21 C23 109.61(17) . .
C16 C21 H21 108.0 . .
C22 C21 H21 108.0 . .
C23 C21 H21 108.0 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C25 C24 C20 110.15(17) . .
C25 C24 C26 110.75(16) . .
C20 C24 C26 114.25(15) . .
C25 C24 H24 107.1 . .
C20 C24 H24 107.1 . .
C26 C24 H24 107.1 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 B1 2.0421(16) .
Ge1 Ge1 2.4105(3) 3_666
Ge1 H1B 1.49(2) .
Ge1 H2B 1.53(2) .
N1 C1 1.3980(19) .
N1 B1 1.4246(19) .
N1 C3 1.4287(18) .
N2 C2 1.3997(19) .
N2 B1 1.427(2) .
N2 C15 1.4356(17) .
C1 C2 1.342(2) .
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 C8 1.398(2) .
C3 C4 1.402(2) .
C4 C5 1.395(2) .
C4 C9 1.511(3) .
C5 C6 1.379(4) .
C5 H5 0.9500 .
C6 C7 1.366(4) .
C6 H6 0.9500 .
C7 C8 1.400(3) .
C7 H7 0.9500 .
C8 C12 1.516(3) .
C9 C10 1.523(3) .
C9 C11 1.528(3) .
C9 H9 1.0000 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C14 1.519(3) .
C12 C13 1.520(3) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.399(2) .
C15 C20 1.402(2) .
C16 C17 1.401(2) .
C16 C21 1.516(2) .
C17 C18 1.371(3) .
C17 H17 0.9500 .
C18 C19 1.381(3) .
C18 H18 0.9500 .
C19 C20 1.394(2) .
C19 H19 0.9500 .
C20 C24 1.518(2) .
C21 C22 1.525(3) .
C21 C23 1.535(3) .
C21 H21 1.0000 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 C25 1.517(3) .
C24 C26 1.524(3) .
C24 H24 1.0000 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
