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_7037834
_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         'C74 H90 N4 Rh2 Sn2'
_chemical_formula_sum            'C74 H90 N4 Rh2 Sn2'
_chemical_formula_weight         1478.69
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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   geom
_audit_creation_date             2015-11-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2015-12-09 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.213(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6300(8)
_cell_length_b                   30.633(3)
_cell_length_c                   11.9259(10)
_cell_measurement_reflns_used    2922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.866
_cell_measurement_theta_min      2.191
_cell_volume                     3092.6(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.964
_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  0.1184
_diffrn_reflns_av_unetI/netI     0.1477
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30195
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         2.496
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.6146
_exptl_absorpt_correction_T_min  0.4880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0921 before and 0.0795 after correction.
The Ratio of minimum to maximum transmission is 0.7940.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.579
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.1046
_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^)+(0.0913P)^2^+88.8895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4279
_reflns_number_total             6896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04060d2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7037826--7037834.cif.'
_cod_database_code               7037834
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.771
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.003
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C30(H30), C31(H31), C34(H34), C35(H35)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C32(H32A,
 H32B), C33(H33A,H33B), C36(H36A,H36B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C20(H20), C21(H21), C22(H22)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              31988
_shelx_hkl_checksum              26554
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'