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_7037742
_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 Ga2 N4 P2 Si2'
_chemical_formula_sum            'C50 H72 Ga2 N4 P2 Si2'
_chemical_formula_weight         986.67
_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                   19.867(2)
_cell_length_b                   17.8620(17)
_cell_length_c                   29.774(3)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.122
_cell_measurement_theta_min      2.280
_cell_volume                     10565.7(18)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            138525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.191
_diffrn_reflns_theta_min         2.280
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.8789.
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    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         11716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+9.9130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8859
_reflns_number_total             11716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03889h2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7037738--7037743.cif.'
_cod_original_cell_volume        10565.4(17)
_cod_database_code               7037742
_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:
 C13(H13), C4(H4), C16(H16), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C3(H3), C24(H24), C26(H26), C25(H25), C44(H44), C31(H31), C2(H2),
 C12(H12), C40(H40), C30(H30), C28(H28), C32(H32), C50(H50), C27(H27), C41(H41),
  C46(H46), C33(H33), C11(H11), C48(H48), C49(H49), C42(H42), C47(H47), C43(H43)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C9(H9A,H9B,
 H9C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C18(H18A,
 H18B,H18C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              60319
_olex2_submission_special_instructions 'No special instructions were received'