Six-coordinate ferric porphyrins containing bidentate N-t-butyl-N-nitrosohydroxylaminato ligands: structure, magnetism, IR spectroelectrochemisty, and reactivity.
Xu, Nan; Christian, Jonathan H.; Dalal, Naresh S.; Abucayon, Erwin G.; Lingafelt, Colin; Powell, Douglas R.; Richter-Addo, George B; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20121–20130; doi:10.1039/c5dt03074a

data_7036962
_publ_section_title
;
 Six-coordinate ferric porphyrins containing bidentate
 N-t-butyl-N-nitrosohydroxylaminato ligands: structure, magnetism, IR
 spectroelectrochemisty, and reactivity.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20121
_journal_page_last               20130
_journal_paper_doi               10.1039/c5dt03074a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H37 Fe N6 O2, C H2 Cl2'
_chemical_formula_sum            'C49 H39 Cl2 Fe N6 O2'
_chemical_formula_weight         870.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.746(3)
_cell_angle_beta                 105.162(3)
_cell_angle_gamma                100.150(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7262(15)
_cell_length_b                   13.217(2)
_cell_length_c                   17.511(3)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.21
_cell_volume                     2113.2(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP (Bruker, 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXS-97 (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.219
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015c)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       prism
_exptl_crystal_F_000             902
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/cyclohexane'
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     401
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6817
_reflns_number_total             8306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03074a2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 7036961--7036963.cif.'
_cod_database_code               7036962
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              65710