Cyclic NHC-stabilized silylphosphinoalanes and -gallanes.
Kapitein, Manuel; Balmer, Markus; Niemeier, Lukas; von Hänisch, Carsten; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6275–6281; doi:10.1039/c5dt03889h

data_7037740
_publ_section_title
;
 Cyclic NHC-stabilized silylphosphinoalanes and -gallanes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6275
_journal_page_last               6281
_journal_paper_doi               10.1039/c5dt03889h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C50 H72 Al2 N4 P2 Si2'
_chemical_formula_sum            'C50 H72 Al2 N4 P2 Si2'
_chemical_formula_weight         901.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-05 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8408(8)
_cell_length_b                   17.8369(8)
_cell_length_c                   29.8764(13)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.212
_cell_measurement_theta_min      2.349
_cell_volume                     10573.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            147162
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.285
_diffrn_reflns_theta_min         2.349
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7399
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1085 before and 0.0598 after correction. The Ratio of minimum to maximum transmission is 0.9551. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.173
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0325
_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/[\s^2^(Fo^2^)+(0.0311P)^2^+7.0034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7838
_reflns_number_total             9594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03889h2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7037738--7037743.cif.'
_cod_database_code               7037740
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C13(H13), C4(H4), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C2(H2), C11(H11), C12(H12), C24(H24), C48(H48), C41(H41), C3(H3),
 C40(H40), C47(H47), C43(H43), C49(H49), C44(H44), C42(H42), C46(H46), C28(H28),
  C34(H34), C26(H26), C25(H25), C32(H32), C27(H27), C30(H30), C33(H33), C31(H31)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C15(H15A,
 H15B,H15C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C22(H22A,H22B,H22C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              38105
_olex2_submission_special_instructions 'No special instructions were received'