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_7046567
_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
'C74 H78 Fe3 N4 O2 P4, C37 H39 Fe N P2, 0.85(C4 H8 O)'
_chemical_formula_sum            'C114.4 H123.8 Fe4 N5 O2.85 P6'
_chemical_formula_weight         2023.60
_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             2017-09-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                103.179(2)
_cell_angle_beta                 113.672(2)
_cell_angle_gamma                106.712(2)
_cell_formula_units_Z            2
_cell_length_a                   18.1733(14)
_cell_length_b                   18.5346(14)
_cell_length_c                   20.2827(15)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      40.027
_cell_measurement_theta_min      2.585
_cell_volume                     5514.3(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1083
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33016
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        40.097
_diffrn_reflns_theta_max         40.10
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.345
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1122 before and 0.0590 after correction. The Ratio of minimum to maximum transmission is 0.8310. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         6720
_refine_ls_number_restraints     2133
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0262P)^2^+40.8093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4715
_reflns_number_total             6720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01761a2.cif
_cod_data_source_block           mqb
_cod_depositor_comments
'Adding full bibliography for 7046563--7046567.cif.'
_cod_original_formula_sum        'C114.40 H123.80 Fe4 N5 O2.85 P6'
_cod_database_code               7046567
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.450
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(N4) = Uanis(C38)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Fixed Sof: O1S(0.85) C2S(0.85) H2SA(0.85) H2SB(0.85) C3S(0.85) H3SA(0.85)
 H3SB(0.85) C4S(0.85) H4SA(0.85) H4SB(0.85) C5S(0.85) H5SA(0.85) H5SB(0.85)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C51(H51A,H51B), C52(H52A,H52B), C87(H87A,
 H87B), C88(H88A,H88B), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB),
 C5S(H5SA,H5SB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86), C90(H90), C91(H91), C92(H92), C93(H93),
 C94(H94), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C106(H10A,H10B,H10C),
 C107(H10D,H10E,H10F), C108(H10G,H10H,H10I), C109(H10J,H10K,H10L), C110(H11A,
 H11B,H11C)
;
_shelx_res_checksum              12488
_shelx_fab_checksum              77127
_olex2_submission_special_instructions 'No special instructions were received'