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_7037741
_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         'C58 H76 Al2 N4 P2 Si2, C4 H10 O'
_chemical_formula_sum            'C62 H86 Al2 N4 O P2 Si2'
_chemical_formula_weight         1075.42
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8684(7)
_cell_length_b                   20.7005(9)
_cell_length_c                   19.0724(9)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.346
_cell_measurement_theta_min      2.644
_cell_volume                     6261.1(5)
_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 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            199865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.988
_diffrn_reflns_theta_min         2.239
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1169 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8806.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.049
_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     682
_refine_ls_number_reflns         15044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0300P)^2^+3.4540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11490
_reflns_number_total             15044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03889h2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7037738--7037743.cif.'
_cod_database_code               7037741
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C21(H21), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C60(H60A,H60B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C38(H38), C57(H57), C14(H14), C55(H55), C36(H36), C13(H13), C32(H32),
 C59(H59), C52(H52), C43(H43), C12(H12), C11(H11), C39(H39), C53(H53), C51(H51),
  C6(H6), C35(H35), C7(H7), C49(H49), C33(H33), C42(H42), C56(H56), C50(H50),
 C40(H40), C5(H5), C34(H34), C58(H58)
2.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C19(H19A,H19B,H19C), C46(H46A,H46B,H46C), C20(H20A,H20B,
 H20C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C45(H45A,H45B,H45C), C28(H28A,
 H28B,H28C), C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C),
 C23(H23A,H23B,H23C), C61(H61A,H61B,H61C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              62962
_olex2_submission_special_instructions 'No special instructions were received'