X-ray Structure and Properties of the Ferrous Octaethylporphyrin Nitroxyl Complex.
Kundakarla, Nagabhushanam; Lindeman, Sergey; Rahman, Md Hafiz; Ryan, Michael D.; Inorganic chemistry 55 (2016) 2070–2075; doi:10.1021/acs.inorgchem.5b02384

data_4346939
_publ_section_title
;
 X-ray Structure and Properties of the Ferrous Octaethylporphyrin Nitroxyl
 Complex.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2070
_journal_page_last               2075
_journal_paper_doi               10.1021/acs.inorgchem.5b02384
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C54 H80 Fe K N7 O7, 0.5(C14 H10)'
_chemical_formula_sum            'C61 H85 Fe K N7 O7'
_chemical_formula_weight         1123.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                83.4024(14)
_cell_angle_beta                 88.8922(12)
_cell_angle_gamma                73.4501(14)
_cell_formula_units_Z            4
_cell_length_a                   14.7775(2)
_cell_length_b                   19.6688(3)
_cell_length_c                   21.2458(3)
_cell_measurement_reflns_used    39948
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0770
_cell_measurement_theta_min      3.2960
_cell_volume                     5879.60(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_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   -124.00 -79.00   1.00    3.00    --  -41.40 -99.00-120.00   45
  2  \w    -71.00  33.00   1.00    3.00    --  -41.40  57.00-120.00  104
  3  \w   -118.00 -15.00   1.00    3.00    --  -41.40 -37.00  90.00  103
  4  \w   -124.00 -79.00   1.00    3.00    --  -41.40 -99.00-180.00   45
  5  \w   -124.00 -79.00   1.00    3.00    --  -41.40 -99.00 150.00   45
  6  \w      1.00  83.00   1.00    3.00    --   41.40 -99.00  60.00   82
  7  \w     23.00  99.00   1.00    3.00    --   41.40-125.00   0.00   76
  8  \w     33.00 122.00   1.00   12.00    --  108.29-125.00  90.00   89
  9  \w     34.00 139.00   1.00   12.00    --  108.29 -61.00 120.00  105
 10  \w     24.00 109.00   1.00   12.00    --  108.29 -94.00 120.00   85
 11  \w     34.00 136.00   1.00   12.00    --  108.29 -45.00   0.00  102
 12  \w     33.00 122.00   1.00   12.00    --  108.29-125.00 -60.00   89
 13  \w     94.00 178.00   1.00   12.00    --  108.29 125.00  30.00   84
 14  \w     81.00 178.00   1.00   12.00    --  108.29  45.00 120.00   97
 15  \w     30.00 139.00   1.00   12.00    --  108.29 -30.00-120.00  109
 16  \w     94.00 178.00   1.00   12.00    --  108.29 125.00 -30.00   84
 17  \w     30.00 142.00   1.00   12.00    --  108.29 -77.00 -90.00  112
 18  \w     47.00 178.00   1.00   12.00    --  108.29  15.00-120.00  131
 19  \w   -124.00 -79.00   1.00    3.00    --  -41.40 -99.00 -30.00   45
 20  \w   -124.00 -79.00   1.00    3.00    --  -41.40 -99.00  30.00   45
 21  \w   -115.00 -12.00   1.00    3.00    --  -41.40 -57.00 -60.00  103
 22  \w   -115.00 -12.00   1.00    3.00    --  -41.40 -57.00  30.00  103
 23  \w   -115.00 -12.00   1.00    3.00    --  -41.40 -57.00-150.00  103
 24  \w     78.00 178.00   1.00   12.00    --  108.29  30.00  60.00  100
 25  \w     78.00 178.00   1.00   12.00    --  108.29  61.00-150.00  100
 26  \w     78.00 178.00   1.00   12.00    --  108.29  30.00 -30.00  100
 27  \w     75.00 178.00   1.00   12.00    --  108.29  77.00 120.00  103
 28  \w     75.00 178.00   1.00   12.00    --  108.29  77.00  60.00  103
 29  \w     81.00 178.00   1.00   12.00    --  108.29  45.00   0.00   97
 30  \w     75.00 178.00   1.00   12.00    --  108.29  77.00 -60.00  103
 31  \w     78.00 178.00   1.00   12.00    --  108.29  61.00-180.00  100
 32  \w     78.00 178.00   1.00   12.00    --  108.29  61.00 -90.00  100
 33  \w     75.00 178.00   1.00   12.00    --  108.29  77.00-120.00  103
 34  \w   -120.00  -8.00   1.00    3.00    --  -41.40 -77.00 150.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0998794000
_diffrn_orient_matrix_UB_12      0.0047006000
_diffrn_orient_matrix_UB_13      0.0137736000
_diffrn_orient_matrix_UB_21      0.0292313000
_diffrn_orient_matrix_UB_22      -0.0160363000
_diffrn_orient_matrix_UB_23      -0.0679536000
_diffrn_orient_matrix_UB_31      -0.0316198000
_diffrn_orient_matrix_UB_32      0.0805322000
_diffrn_orient_matrix_UB_33      -0.0228453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            111300
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.148
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1392
_refine_ls_number_reflns         23568
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+7.9470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                18739
_reflns_number_total             23568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02384_si_001.cif
_cod_data_source_block           ryann
_cod_original_cell_volume        5879.61(16)
_cod_database_code               4346939
_chemical_oxdiff_formula         'C36 H44 Cl Fe N4 C18 N2 H36 O6 K'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Same fragment restrains
{C1S, C2S, C3S, C4S, C5S, C6S, C7S} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1Q, C2Q, C3Q, C4Q, C5Q, C6Q, C7Q}
{C1S, C2S, C3S, C4S, C5S, C6S, C7S} sigma for 1-2: 0.02, 1-3: 0.04
as
{C8Q, C9Q, C10Q, C11Q, C12Q, C13Q, C14Q}
3. Others
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(C21A)=Sof(H21B)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Fixed Sof: C1Q(0.5) H1Q(0.5) C2Q(0.5) C3Q(0.5) H3Q(0.5) C4Q(0.5) H4Q(0.5)
 C5Q(0.5) H5Q(0.5) C6Q(0.5) H6Q(0.5) C7Q(0.5) C8Q(0.5) H8Q(0.5) C9Q(0.5)
 C10Q(0.5) H10Q(0.5) C11Q(0.5) H11Q(0.5) C12Q(0.5) H12Q(0.5) C13Q(0.5)
 H13Q(0.5) C14Q(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21E,H21F), C23(H23C,H23D), C25(H25C,H25D), C27(H27C,H27D), C29(H29E,
 H29F), C31(H31C,H31D), C33(H33C,H33D), C35(H35C,H35D), C37(H37C,H37D),
 C38(H38C,H38D), C39(H39C,H39D), C40(H40C,H40D), C41(H41C,H41D), C42(H42C,H42D),
  C43(H43C,H43D), C44(H44C,H44D), C45(H45C,H45D), C46(H46C,H46D), C47(H47C,
 H47D), C48(H48C,H48D), C49(H49C,H49D), C50(H50C,H50D), C51(H51C,H51D),
 C52(H52C,H52D), C53(H53C,H53D), C54(H54C,H54D), C21A(H21B,H21A), C21B(H21C,
 H21D), C23A(H23A,H23B), C25A(H25A,H25B), C27A(H27A,H27B), C29A(H29A,H29B),
 C29A(H29C,H29D), C31A(H31A,H31B), C33A(H33A,H33B), C35A(H35A,H35B), C37A(H37A,
 H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B), C41A(H41A,H41B),
 C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,H44B), C45A(H45A,H45B), C46A(H46A,
 H46B), C47A(H47A,H47B), C48A(H48A,H48B), C49A(H49A,H49B), C50A(H50A,H50B),
 C51A(H51A,H51B), C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15), C20(H20), C5A(H5A), C10A(H10A), C15A(H15A),
 C20A(H20A), C1S(H1S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C1Q(H1Q),
 C3Q(H3Q), C4Q(H4Q), C5Q(H5Q), C6Q(H6Q), C8Q(H8Q), C10Q(H10Q), C11Q(H11Q),
 C12Q(H12Q), C13Q(H13Q)
4.c Idealised Me refined as rotating group:
 C22(H22G,H22H,H22I), C24(H24D,H24E,H24F), C26(H26D,H26E,H26F), C28(H28D,H28E,
 H28F), C30(H30G,H30H,H30I), C32(H32D,H32E,H32F), C34(H34D,H34E,H34F), C36(H36D,
 H36E,H36F), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C24A(H24A,H24B,H24C),
 C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C32A(H32A,H32B,H32C), C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C)
;
_olex2_date_sample_data_collection 2015-04-30
_olex2_date_sample_submission    2015-04-29
_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 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.420