Assembly of NHC-stabilized 2-hydrophosphasilenes from Si(iv) precursors: a Lewis acid-base complex.
Dhara, Debabrata; Mandal, Debdeep; Maiti, Avijit; Yildiz, Cem B.; Kalita, Pankaj; Chrysochos, Nicolas; Schulzke, Carola; Chandrasekhar, Vadapalli; Jana, Anukul; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19290–19298; doi:10.1039/c6dt04321f

data_7041210
_publ_section_title
;
 Assembly of NHC-stabilized 2-hydrophosphasilenes from Si(iv) precursors:
 a Lewis acid-base complex.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19290
_journal_page_last               19298
_journal_paper_doi               10.1039/c6dt04321f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C58 H85 N2 P Si, 2(C6 H6)'
_chemical_formula_sum            'C70 H97 N2 P Si'
_chemical_formula_weight         1025.55
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-27 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.508(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.327(4)
_cell_length_b                   14.765(3)
_cell_length_c                   21.810(4)
_cell_measurement_reflns_used    6578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.37
_cell_volume                     6276(2)
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76230
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.697
_diffrn_reflns_theta_min         1.931
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1172 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.8334.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0580P)^2^+0.9025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8026
_reflns_number_total             12984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04321f2.cif
_cod_data_source_block           vc_aj_dd_4
_cod_depositor_comments
'Adding full bibliography for 7041209--7041210.cif.'
_cod_original_cell_volume        6275.8(19)
_cod_database_code               7041210
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 Si1(H1), C13(H13), C28(H28), C19(H19), C34(H34), C43(H43), C16(H16), C49(H49),
  C31(H31), C46(H46)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5), C24(H24), C9(H9), C26(H26), C11(H11), C39(H39),
 C41(H41), C64(H64), C69(H69), C67(H67), C70(H70), C68(H68), C62(H62), C63(H63),
  C65(H65), C61(H61), C71(H71), C72(H72), C66(H66)
2.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C14(H14A,H14B,H14C), C57(H57A,H57B,H57C), C29(H29A,H29B,
 H29C), C47(H47A,H47B,H47C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C30(H30A,
 H30B,H30C), C44(H44A,H44B,H44C), C58(H58A,H58B,H58C), C15(H15A,H15B,H15C),
 C59(H59A,H59B,H59C), C18(H18A,H18B,H18C), C51(H51A,H51B,H51C), C36(H36A,H36B,
 H36C), C45(H45A,H45B,H45C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C32(H32A,
 H32B,H32C), C17(H17A,H17B,H17C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              35084
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'