Manganese catalysed dehydrocoupling of silanes and siloxanes with ammonia to prepare oligosilazanes and polysiloxazanes.
Mehta, Gautam K.; Nguyen, Thao T.; Flores, Marco; Trovitch, Ryan J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14272–14277; doi:10.1039/d4dt01982b

data_7716750
_publ_section_title
;
 Manganese catalysed dehydrocoupling of silanes and siloxanes with ammonia
 to prepare oligosilazanes and polysiloxazanes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14272
_journal_page_last               14277
_journal_paper_doi               10.1039/d4dt01982b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C58 H86 Mn2 N6'
_chemical_formula_sum            'C58 H86 Mn2 N6'
_chemical_formula_weight         977.20
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-04-18 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.125(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.875(10)
_cell_length_b                   14.747(7)
_cell_length_c                   16.257(7)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      24.2437
_cell_measurement_theta_min      2.5062
_cell_volume                     5483(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS, 2014)'
_computing_data_collection       'Bruker Instrument Service V2015.5.1.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2014)'
_computing_molecular_graphics    'XShell V6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 V2014.11-0 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT V2014/4 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22437
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS, 2014)'
_exptl_crystal_colour            'clear light yellow-green'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0646P)^2^+2.5674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                3954
_reflns_number_total             4996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01982b2.cif
_cod_data_source_block           Nguyen_3_063_3
_cod_depositor_comments          'Adding full bibliography for 7716750.cif.'
_cod_original_cell_volume        5483.(4)
_cod_database_code               7716750
_shelx_res_checksum              62377
_shelx_hkl_checksum              78411