Vanadyl β-tetrabromoporphyrin: synthesis, crystal structure and its use as an efficient and selective catalyst for olefin epoxidation in aqueous medium
Dar, Tawseef Ahmad; Tomar, Reshu; Mian, Rasel Mohammad; Sankar, Muniappan; Maurya, Mannar Ram; RSC Advances 9 (2019) 10405–; doi:10.1039/C8RA09825E

data_7232562
_publ_section_title
;
 Vanadyl \b-tetrabromoporphyrin: synthesis, crystal structure and its use
 as an efficient and selective catalyst for olefin epoxidation in aqueous
 medium
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10405
_journal_paper_doi               10.1039/C8RA09825E
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         '0.5(C88 H48 Br8 N8 O V2)'
_chemical_formula_sum            'C44 H24 Br4 N4 O0.5 V'
_chemical_formula_weight         987.26
_chemical_name_common            'Tetrabromovanadylporphyrin dimer'
_chemical_name_systematic
'2,3,12,13-bromo-5,10,15,20-tetraphenylporphyrinatovanadium ?-oxodimer'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_audit_creation_date             2018-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-19 deposited with the CCDC.    2019-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.719(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.844(9)
_cell_length_b                   13.822(4)
_cell_length_c                   19.654(7)
_cell_measurement_reflns_used    12130
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.210
_cell_measurement_theta_min      0.72
_cell_volume                     7723(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.9935
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21499
_diffrn_reflns_theta_full        18.2126
_diffrn_reflns_theta_max         18.21
_diffrn_reflns_theta_min         0.72
_exptl_absorpt_coefficient_mu    4.435
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Brucker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.6981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3859.2129
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/Chloroform/methanol'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.8679
_refine_diff_density_min         -0.6394
_refine_diff_density_rms         0.1639
_refine_ls_d_res_high            1.1370
_refine_ls_d_res_low             28.4286
_refine_ls_goodness_of_fit_ref   1.0924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    96
_refine_ls_number_parameters     619
_refine_ls_number_reflns         5465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0924
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.0018
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+22.8728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -26
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3875
_reflns_number_total             5465
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra09825e2.cif
_cod_data_source_block           shelx
_cod_database_code               7232562
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C47(H47), C73(H73), C25(H25), C3(H3), C46(H46), C2(H2), C66(H66), C68(H68),
 C74(H74), C36(H36), C049(H049), C26(H26), C57(H57), C12(H12), C34(H34),
 C35(H35), C066(H066), C78(H78), C79(H79), C69(H69), C81(H81), C85(H85),
 C40(H40), C67(H67), C31(H31), C70(H70), C30(H30), C13(H13), C082(H082),
 C83(H83), C80(H80), C56(H56), C87(H87), C38(H38), C72(H72), C090(H090),
 C28(H28), C86(H86), C29(H29), C76(H76), C27(H27), C23(H23), C22(H22), C84(H84),
  C82(H82), C24(H24), C75(H75), C37(H37)
;
_olex2_submission_special_instructions 'No special instructions were received'