A Ni(I)Fe(II) analogue of the Ni-L state of the active site of the [NiFe] hydrogenases
Carlo U. Perotto; George Marshall; Graham J. Jones; E. Stephen Davies; William Lewis; Jonathan McMaster; Martin Schroder; Chem.Commun. 51 (2015) 16988–; doi:10.1039/C5cc05881C

data_7118090
_publ_section_title
;
 A Ni(I)Fe(II) analogue of the Ni-L state of the active site of the [NiFe]
 hydrogenases
;
_journal_name_full               Chem.Commun.
_journal_page_first              16988
_journal_paper_doi               10.1039/C5cc05881C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C31 H60 Fe N6 Ni S2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C33 H63 F12 Fe N7 Ni P2 S2'
_chemical_formula_weight         1026.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9779(2)
_cell_length_b                   15.33320(16)
_cell_length_c                   25.33735(19)
_cell_measurement_reflns_used    46493
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2100
_cell_measurement_theta_min      2.8790
_cell_volume                     9703.98(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -45.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000   60.0000 57

  2 omega   -7.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  -60.0000 26

  3 omega   19.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   57.0000   60.0000 90

  4 omega   26.00  105.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   30.0000 79

  5 omega   27.00  144.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000 -150.0000 117

  6 omega   41.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000    0.0000 57

  7 omega  -29.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573  -77.0000  -90.0000 102

  8 omega   13.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   77.0000  150.0000 101

  9 omega  -26.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573  -57.0000  150.0000 94

 10 omega   18.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   57.0000  -60.0000 93

 11 omega   84.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000 -120.0000 94

 12 omega   73.00  174.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000    0.0000 101

 13 omega   82.00  174.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -30.0000 92

 14 omega   35.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   60.0000 63

 15 omega  -92.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   30.0000 90

 16 omega   18.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   57.0000  120.0000 93

 17 omega   22.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   37.0000  -90.0000 92

 18 omega   13.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   77.0000  -30.0000 101

 19 omega   74.00  124.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000   90.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0607248000
_diffrn_orient_matrix_UB_12      0.0153715000
_diffrn_orient_matrix_UB_13      -0.0052706000
_diffrn_orient_matrix_UB_21      -0.0048186000
_diffrn_orient_matrix_UB_22      0.0064625000
_diffrn_orient_matrix_UB_23      0.0604874000
_diffrn_orient_matrix_UB_31      0.0097722000
_diffrn_orient_matrix_UB_32      0.0990576000
_diffrn_orient_matrix_UB_33      -0.0031338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89937
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.334
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.000
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.6628
_exptl_crystal_size_mid          0.1498
_exptl_crystal_size_min          0.0708
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9779
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+7.7066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9206
_reflns_number_total             9779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05881c2.cif
_cod_data_source_block           nicplw
_cod_original_cell_volume        9704.00(15)
_cod_database_code               7118090
_nottingham_internal_coll_name   NICPLW
_nottingham_internal_coll_number 13771
_nottingham_internal_coll_client CP/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '15.0000, 60.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxcp1
_nottingham_internal_coll_date   03/07/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 04/07/2014
_nottingham_internal_process_user pczcp1
_nottingham_internal_solution_date 05/07/2014
_nottingham_internal_solution_user pczcp1
_nottingham_internal_refinement_date 08/07/2014
_nottingham_internal_refinement_user pczcp1
_nottingham_internal_validation_date 5/3/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 5/3/2015
_chemical_oxdiff_formula         'C33 H63 F11 Fe1 N7 Ni1 P2 S2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N7, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F1, F1A, F2, F2A, F3, F3A, F4, F4A, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'