Ligand-Based Reduction of Nitrate to Nitric Oxide Utilizing a Proton-Responsive Secondary Coordination Sphere.
Delgado, Mayra; Gilbertson, John D.; Chem. Commun.  (2017) –; doi:10.1039/C7CC06541H

data_7120710
_publ_section_title
;
 Ligand-Based Reduction of Nitrate to Nitric Oxide Utilizing a
 Proton-Responsive Secondary Coordination Sphere.
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06541H
_journal_year                    2017
_chemical_formula_moiety         'C29 H44 Fe N6 O2, F6 P'
_chemical_formula_sum            'C29 H44 F6 Fe N6 O2 P'
_chemical_formula_weight         709.52
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-26
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.03.02 svn.r3394 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2017-08-20 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                80.311(4)
_cell_angle_beta                 85.323(3)
_cell_angle_gamma                78.583(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3541(4)
_cell_length_b                   12.2825(6)
_cell_length_c                   16.8758(6)
_cell_measurement_reflns_used    12483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4800
_cell_measurement_theta_min      2.5570
_cell_volume                     1671.05(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector                 'Pilatus P200K HPC detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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    -78.00  54.00   0.50   15.00    --    0.00 -10.00 144.00  264
  2  \w    -33.00  87.00   0.50   15.00    --    0.00  82.00 -36.00  240
  3  \w    -13.50  76.50   0.50   15.00    --    0.00  63.00  72.00  180
  4  \w      2.00  47.00   0.50   15.00    --    0.00   9.00-180.00   90
  5  \w    -38.50  15.00   0.50   15.00    --    0.00   9.00 -36.00  107
;
_diffrn_measurement_device       'ROD XtaLABPRO'
_diffrn_measurement_device_type  'ROD XtaLABPRO'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0708278000
_diffrn_orient_matrix_UB_12      -0.0428290000
_diffrn_orient_matrix_UB_13      0.0004061000
_diffrn_orient_matrix_UB_21      0.0111056000
_diffrn_orient_matrix_UB_22      0.0044838000
_diffrn_orient_matrix_UB_23      0.0404705000
_diffrn_orient_matrix_UB_31      -0.0488019000
_diffrn_orient_matrix_UB_32      -0.0412644000
_diffrn_orient_matrix_UB_33      0.0135862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27521
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Mo fine focus sealdet ube with SHINE'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0386P)^2^+0.4231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6573
_reflns_number_total             7556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06541h2.cif
_cod_data_source_block           er_proc
_cod_database_code               7120710
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C29 H45 Fe F6 P N6 O2'
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C12(H12), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C6(H6), C21(H21), C4(H4), C22(H22), C5(H5)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C28(H28A,H28B,H28C), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C),
 C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C14(H14A,H14B,
 H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.749