Bridging cyanides from cyanoiron metalloligands to redox-active dinitrosyl iron units.
Ghosh, Pokhraj; Quiroz, Manuel; Pulukkody, Randara; Bhuvanesh, Nattamai; Darensbourg, Marcetta Y.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11812–11819; doi:10.1039/c8dt01761a

data_7046563
_publ_section_title
;
 Bridging cyanides from cyanoiron metalloligands to redox-active
 dinitrosyl iron units.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11812
_journal_page_last               11819
_journal_paper_doi               10.1039/c8dt01761a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C58 H65 Fe2 N5 O2 P2, B F4, C4 H8 O'
_chemical_formula_sum            'C62 H73 B F4 Fe2 N5 O3 P2'
_chemical_formula_weight         1196.70
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.996(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1283(8)
_cell_length_b                   15.3003(5)
_cell_length_c                   23.5487(8)
_cell_measurement_reflns_used    9737
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      61.787
_cell_measurement_theta_min      3.482
_cell_volume                     7353.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex3 (Bruker 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1564
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            126475
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        49.999
_diffrn_reflns_theta_max         49.999
_diffrn_reflns_theta_min         3.481
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_T_max  0.7320
_exptl_absorpt_correction_T_min  0.5006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1517 before and 0.0853 after correction.
The Ratio of minimum to maximum transmission is 0.6839.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       needle
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+59.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6070
_reflns_number_total             7546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01761a2.cif
_cod_data_source_block           fe5mecntnic_sq
_cod_depositor_comments
'Adding full bibliography for 7046563--7046567.cif.'
_cod_database_code               7046563
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.300
_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. Restrained distances
 P1-C31A \\sim P1-C31
 with sigma of 0.02
 P1-C25A \\sim P1-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C31A \\sim
C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.02
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C25A \\sim C26A
\\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim P1: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 P1, C31, C32, C33, C34, C35, C36, C31A, C32A, C33A, C34A, C35A, C36A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 P1, C25, C26, C27, C28, C29, C30, C25A, C26A, C27A, C28A, C30A, C29A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(2)
 Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29)=Sof(C30)=Sof(H30)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C23(H23A,H23B), C24(H24A,H24B), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C15(H15), C17(H17), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
6.c Fitted hexagon refined as free rotating group:
 C25(C26,C27,C28,C29,C30), C25A(C26A,C27A,C28A,C29A,C30A), C31(C32,C33,C34,C35,
 C36), C31A(C32A,C33A,C34A,C35A,C36A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              86069
_shelx_fab_checksum              82423
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'