Synthesis and Reactivity Studies of a Tin(II) Corrole Complex.
Yun, Lin; Vazquez-Lima, Hugo; Fang, Huayi; Yao, Zhengmin; Geisberger, Georg; Dietl, Christian; Ghosh, Abhik; Brothers, Penelope J.; Fu, Xuefeng; Inorganic chemistry 53 (2014) 7047–7054; doi:10.1021/ic501103c

data_4339997
_publ_section_title
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 Synthesis and Reactivity Studies of a Tin(II) Corrole Complex.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7047
_journal_page_last               7054
_journal_paper_doi               10.1021/ic501103c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C41 H15 F15 N4 O2 Sn, C3 H6 O'
_chemical_formula_sum            'C44 H21 F15 N4 O3 Sn'
_chemical_formula_weight         1057.34
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2014-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.707(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5000(18)
_cell_length_b                   26.912(7)
_cell_length_c                   23.054(6)
_cell_measurement_reflns_used    14116
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4852
_cell_measurement_theta_min      1.1653
_cell_volume                     4638(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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
;
'XS (Sheldrick, 2008)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0196
_diffrn_orient_matrix_UB_12      0.1232
_diffrn_orient_matrix_UB_13      0.0483
_diffrn_orient_matrix_UB_21      0.0351
_diffrn_orient_matrix_UB_22      0.0089
_diffrn_orient_matrix_UB_23      -0.0085
_diffrn_orient_matrix_UB_31      -0.0134
_diffrn_orient_matrix_UB_32      0.0166
_diffrn_orient_matrix_UB_33      -0.0379
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31647
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         1.513
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0842
_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^)+(0.0659P)^2^+13.2043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8955
_reflns_number_total             10606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501103c_si_002.cif
_cod_data_source_block           (TPFC)Sn-CH2CH2COOCH3
_cod_depositor_comments
'Adding full bibliography for 4339997--4339999.cif.'
_cod_database_code               4339997
_shelxl_version_number           2013-4
_diffrn_number_total             10862
_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 Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C13(H13), C14(H14), C24(H24), C25(H25), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              33624
_shelx_hkl_checksum              32404
_shelx_fab_checksum              27980