A Cu4S model for the nitrous oxide reductase active sites supported only by nitrogen ligands
Johnson, Brittany J.; Antholine, William E.; Lindeman, Sergey V.; Mankad, Neal P.; Chemical Communications (Cambridge, United Kingdom) 51 (2015) 11860–11863; doi:10.1039/c5cc04675k

data_7117608
_publ_section_title
;
 A Cu4S model for the nitrous oxide reductase active sites supported only
 by nitrogen ligands
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   59
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              11860
_journal_page_last               11863
_journal_paper_doi               10.1039/c5cc04675k
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C76 H92 Cu4 N8 S'
_chemical_formula_sum            'C76 H92 Cu4 N8 S'
_chemical_formula_weight         1403.80
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-04 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   21.82156(6)
_cell_length_b                   21.82156(6)
_cell_length_c                   21.82156(6)
_cell_measurement_reflns_used    38038
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0380
_cell_measurement_theta_min      4.0180
_cell_volume                     10391.00(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     14.00  82.00   1.00    1.00    --   41.52 -99.00 -90.00   68
  2  \w     28.00  68.00   1.00    1.00    --   41.52-125.00-150.00   40
  3  \w     54.00 128.00   1.00    3.00    --  108.29 -61.00-120.00   74
  4  \w     89.00 120.00   1.00    3.00    --  108.29-125.00-120.00   31
  5  \w     58.00  84.00   1.00    3.00    --  108.29-112.00 -97.00   26
  6  \w     34.00  60.00   1.00    3.00    --  108.29-125.00-120.00   26
  7  \w     25.00 105.00   1.00    3.00    --  108.29 -94.00 -90.00   80
  8  \w     51.00 136.00   1.00    3.00    --  108.29 -77.00  30.00   85
  9  \w     83.00 141.00   1.00    3.00    --  108.29 -77.00  90.00   58
 10  \w     45.00 122.00   1.00    3.00    --  108.29-125.00  60.00   77
 11  \w     30.00 133.00   1.00    3.00    --  108.29 -30.00   0.00  103
 12  \w     82.00 140.00   1.00    3.00    --  108.29  45.00-120.00   58
 13  \w    143.00 169.00   1.00    3.00    --  108.29  45.00-180.00   26
 14  \w     81.00 131.00   1.00    3.00    --  108.29  45.00-180.00   50
 15  \w     28.00 159.00   1.00    3.00    --  108.29 -15.00-150.00  131
 16  \w    -65.00  32.00   1.00    1.00    --  -41.52  57.00 150.00   97
 17  \w   -110.00 -18.00   1.00    1.00    --  -41.52 -57.00   0.00   92
 18  \w   -118.00 -93.00   1.00    1.00    --  -41.52 -99.00 -60.00   25
 19  \w   -123.00 -81.00   1.00    1.00    --  -41.52 -99.00  90.00   42
 20  \w   -122.00 -89.00   1.00    1.00    --  -41.52 -99.00 150.00   33
;
_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      -0.0175036000
_diffrn_orient_matrix_UB_12      0.0437035000
_diffrn_orient_matrix_UB_13      0.0525860000
_diffrn_orient_matrix_UB_21      -0.0299013000
_diffrn_orient_matrix_UB_22      -0.0537196000
_diffrn_orient_matrix_UB_23      0.0346848000
_diffrn_orient_matrix_UB_31      0.0615483000
_diffrn_orient_matrix_UB_32      -0.0137869000
_diffrn_orient_matrix_UB_33      0.0317815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78257
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.22
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.028
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.622
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0419P)^2^+1.9688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                3467
_reflns_number_total             3548
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7117486
_cod_data_source_file            c5cc04675k2.cif
_cod_data_source_block           neal1pa
_cod_original_cell_volume        10391.01(5)
_cod_database_code               7117608
_chemical_oxdiff_formula         'Cu4 S2 N8 C76 H92'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.511(17) 0.489(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Cu1A(0.5) Cu1B(0.5) S1(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C13(H13), C15(H15)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_olex2_date_sample_data_collection 2015-04-28
_olex2_date_sample_submission    2015-04-27
_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 1.771
_oxdiff_exptl_absorpt_empirical_full_min 0.725