Synthesis and characterization of antimony(V)-oxo corrole complexes
Mondal, Sruti; Garai, Antara; Naik, Pratyush Kumar; Adha, Jogesh Kumar; Kar, Sanjib; Inorganica Chimica Acta 501 (2020) 119300–; doi:10.1016/j.ica.2019.119300

data_1565618
_publ_section_title
;
 Synthesis and characterization of antimony(V)-oxo corrole complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119300
_journal_paper_doi               10.1016/j.ica.2019.119300
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C37 H23 N4 Sb'
_chemical_formula_sum            'C37 H21 N4 Sb'
_chemical_formula_weight         643.33
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 99.256(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4741(8)
_cell_length_b                   21.8912(10)
_cell_length_c                   10.7274(6)
_cell_measurement_reflns_used    8212
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.6340
_cell_measurement_theta_min      3.6280
_cell_volume                     2891.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     13.00  45.00   0.50  100.00    --    1.86-116.00 -55.00   64
  2  \w     -5.00  20.00   0.50  100.00    --   -2.33-116.00 -55.00   50
  3  \w    -33.00  -8.00   0.50  100.00    --    1.86 -38.00 -30.00   50
  4  \w      0.00  26.00   0.50  100.00    --    1.86 -99.00 -60.00   52
  5  \w    -65.00  -5.00   0.50  100.00    --    1.86 -19.00-120.00  120
  6  \w      7.00  67.00   0.50  100.00    --    1.86  38.00 150.00  120
  7  \w     -6.00  32.00   0.50  100.00    --   -2.33 -99.00-180.00   76
  8  \w      0.00  62.00   0.50  100.00    --   -2.33  38.00  30.00  124
  9  \w    -19.00  11.00   0.50  100.00    --   -2.33 -99.00 120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113861000
_diffrn_orient_matrix_UB_12      -0.0316560000
_diffrn_orient_matrix_UB_13      0.0070773000
_diffrn_orient_matrix_UB_21      0.0520034000
_diffrn_orient_matrix_UB_22      0.0048980000
_diffrn_orient_matrix_UB_23      -0.0170054000
_diffrn_orient_matrix_UB_31      0.0220450000
_diffrn_orient_matrix_UB_32      0.0047747000
_diffrn_orient_matrix_UB_33      0.0644137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32351
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1288
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+1.1056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4427
_reflns_number_total             6112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-501-119300.cif
_cod_data_source_block           2
_cod_database_code               1565618
_chemical_oxdiff_formula         'C H N O Sb'
_diffrn_oxdiff_ac3_digest_frames
;
011aad297b55dcb0926d7018ff79da9140000250faf
;
_diffrn_oxdiff_ac3_digest_hkl
;
016724a9420c0a84952fcf3358a3644fdb15cf
;
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00C(H00C), C00I(H00I), C00N(H00N), C00P(H00P), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C013(H013), C015(H015), C017(H017), C018(H018)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.695