Synthetic, structural and reaction chemistry of N-heterocyclic germylene and stannylene compounds featuring N-boryl substituents.
Kristinsdóttir, Lilja; Oldroyd, Nicola L.; Grabiner, Rachel; Knights, Alastair W.; Heilmann, Andreas; Protchenko, Andrey V.; Niu, Haoyu; Kolychev, Eugene L.; Campos, Jesús; Hicks, Jamie; Christensen, Kirsten E.; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11951–11960; doi:10.1039/c9dt02449b

data_7701710
_publ_section_title
;
 Synthetic, structural and reaction chemistry of N-heterocyclic germylene
 and stannylene compounds featuring N-boryl substituents.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11951
_journal_page_last               11960
_journal_paper_doi               10.1039/c9dt02449b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H83 B2 Ge N7 O2, 0.5(C5 H12)'
_chemical_formula_sum            'C62.5 H89 B2 Ge N7 O2'
_chemical_formula_weight         1064.61
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-09 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   42.2093(12)
_cell_length_b                   42.2093(12)
_cell_length_c                   13.8670(5)
_cell_measurement_reflns_used    6539
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.1520
_cell_measurement_theta_min      3.9170
_cell_volume                     24705.8(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35614
_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         76.416
_diffrn_reflns_theta_min         3.956
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       needle
_exptl_crystal_F_000             9136
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12758
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0797P)^2^+29.0843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9904
_reflns_number_total             12758
_reflns_threshold_expression     'I > 2\s(I)'
_oxford_structure_analysis_title 195rgek17
_cod_data_source_file            c9dt02449b2.cif
_cod_data_source_block           (L2)Ge(C5H4NO)(OH)
_cod_original_cell_volume        24705.8(17)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C62.50 H89 B2 Ge N7 O2'
_cod_database_code               7701710
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              10277