Synthesis and reactivity of fluorenyl-tethered N-heterocyclic stannylenes.
Roselló-Merino, Marta; Mansell, Stephen M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6282–6293; doi:10.1039/c5dt04060d

data_7037828
_publ_section_title
;
 Synthesis and reactivity of fluorenyl-tethered N-heterocyclic
 stannylenes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6282
_journal_page_last               6293
_journal_paper_doi               10.1039/c5dt04060d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '4(C42 H59.25 N4 O1.5), 2(H4 O2), Cl'
_chemical_formula_sum            'C168 H245 Cl N16 O10'
_chemical_formula_weight         2684.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-09-14 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.437(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   34.733(3)
_cell_length_b                   5.8657(5)
_cell_length_c                   19.4635(17)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.79
_cell_volume                     3803.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11915
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.746
_diffrn_reflns_theta_max         24.746
_diffrn_reflns_theta_min         1.091
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.7093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0765 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.9520.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+2.9746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2478
_reflns_number_total             3205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04060d2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7037826--7037834.cif.'
_cod_database_code               7037828
_olex2_refinement_description
;
1. Shared sites
{H2NA, H2NB}
{H4NB, H4NA}
2. Others
 Fixed Sof: H1N(0.5) H2NA(0.5) H2NB(0.0625) H3N(0.5) H4NA(0.5) H4NB(0.0625)
 H1W(0.5) H2W(0.5) O2(0.75) H3W(0.5) H4W(0.5) H5W(0.5) Cl1(0.125)
 Fixed U12: O1(0)
 Fixed U23: O1(0)
 Fixed Uiso: H1N(0.042) H2NA(0.042) H2NB(0.042) H3N(0.043) H4NA(0.043)
 H4NB(0.043) H1(0.025) H3(0.026) H4(0.028) H5(0.027) H6(0.024) H9(0.025)
 H10(0.028) H11(0.03) H12(0.027) H14A(0.028) H14B(0.028) H15A(0.032)
 H15B(0.032) H16A(0.034) H16B(0.034) H17A(0.037) H17B(0.037) H19A(0.05)
 H19B(0.05) H19C(0.05) H20A(0.046) H20B(0.046) H20C(0.046) H21A(0.056)
 H21B(0.056) H21C(0.056) H1W(0.055) H2W(0.055) H3W(0.072) H4W(0.072) H5W(0.072)
 Fixed X: H1(0.3277) H3(0.3419) H4(0.3142) H5(0.28) H6(0.2718) H9(0.2693)
 H10(0.2735) H11(0.3076) H12(0.3377) H14A(0.3942) H14B(0.3948) H15A(0.3944)
 H15B(0.3976) H16A(0.463) H16B(0.4534) H17A(0.5253) H17B(0.5156) H19A(0.5927)
 H19B(0.6261) H19C(0.592) H20A(0.5641) H20B(0.6095) H20C(0.577) H21A(0.5707)
 H21B(0.6055) H21C(0.56) O1(0.5) Cl1(0.5)
 Fixed Y: H1(1.1722) H3(1.0447) H4(0.7829) H5(0.4608) H6(0.3988) H9(0.4109)
 H10(0.4975) H11(0.821) H12(1.069) H14A(1.1218) H14B(1.1046) H15A(0.6965)
 H15B(0.724) H16A(0.5066) H16B(0.4838) H17A(0.678) H17B(0.6757) H19A(0.4092)
 H19B(0.4443) H19C(0.6329) H20A(0.0109) H20B(0.071) H20C(0.0315) H21A(0.6037)
 H21B(0.4205) H21C(0.3594) Cl1(1)
 Fixed Z: H1(0.2623) H3(0.4143) H4(0.4782) H5(0.4216) H6(0.2993) H9(0.1608)
 H10(0.0457) H11(0.0255) H12(0.1202) H14A(0.2539) H14B(0.3362) H15A(0.3259)
 H15B(0.2459) H16A(0.2838) H16B(0.3594) H17A(0.3396) H17B(0.4154) H19A(0.3386)
 H19B(0.4136) H19C(0.3853) H20A(0.4536) H20B(0.4569) H20C(0.3811) H21A(0.4985)
 H21B(0.5289) H21C(0.5248) O1(0.25) Cl1(0.5)
;
_shelx_res_checksum              4244
_shelx_hkl_checksum              89750
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'