Phosphane-functionalized heavier tetrylenes: synthesis of silylene- and germylene-decorated phosphanes and their reactions with Group 10 metal complexes.
Cabeza, Javier A.; García-Álvarez, Pablo; Laglera-Gándara, Carlos J; Pérez-Carreño, Enrique; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8331–8339; doi:10.1039/d0dt01727b

data_7704536
_publ_section_title
;
 Phosphane-functionalized heavier tetrylenes: synthesis of silylene- and
 germylene-decorated phosphanes and their reactions with Group 10 metal
 complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8331
_journal_page_last               8339
_journal_paper_doi               10.1039/d0dt01727b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H46 N3 P Si'
_chemical_formula_sum            'C28 H46 N3 P Si'
_chemical_formula_weight         483.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.564(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   18.065(5)
_cell_length_c                   18.265(5)
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_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.51
_cell_volume                     2905(2)
_computing_cell_refinement       'BRUKER APEX3'
_computing_data_collection       'BRUKER APEX3'
_computing_data_reduction        'BRUKER APEX3'
_computing_molecular_graphics
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2019)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0274
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         2.237
_diffrn_source                   'Incoatec high brillance I\muS microsource'
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_exptl_absorpt_correction_T_max  0.7371
_exptl_absorpt_correction_T_min  0.7085
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; 
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 

Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            orange
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_exptl_crystal_size_min          0.093
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_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0502
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.1423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0985
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_reflns_number_gt                6123
_reflns_number_total             7251
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           1Si
_cod_depositor_comments
'Adding full bibliography for 7704536--7704539.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704536
_shelxl_version_number           2014-3
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