Assembly, Structure, and Reactivity of Cu4S and Cu3S Models for the Nitrous Oxide Reductase Active Site, CuZ*.
Johnson, Brittany J.; Lindeman, Sergey V.; Mankad, Neal P.; Inorganic chemistry 53 (2014) 10611–10619; doi:10.1021/ic501720h

data_4341476
_publ_section_title
;
 Assembly, Structure, and Reactivity of Cu4S and Cu3S Models for the
 Nitrous Oxide Reductase Active Site, CuZ*.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10611
_journal_page_last               10619
_journal_paper_doi               10.1021/ic501720h
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C72 H63 Cu3 I N3 P6 S'
_chemical_formula_sum            'C72 H63 Cu3 I N3 P6 S'
_chemical_formula_weight         1505.65
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                108.460(2)
_cell_angle_beta                 90.8367(19)
_cell_angle_gamma                118.571(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7161(3)
_cell_length_b                   13.9702(4)
_cell_length_c                   20.5980(5)
_cell_measurement_reflns_used    25086
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5740
_cell_measurement_theta_min      3.7490
_cell_volume                     3221.96(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0001311000
_diffrn_orient_matrix_UB_12      -0.0060403000
_diffrn_orient_matrix_UB_13      -0.0759844000
_diffrn_orient_matrix_UB_21      0.0000238000
_diffrn_orient_matrix_UB_22      -0.1160838000
_diffrn_orient_matrix_UB_23      -0.0209997000
_diffrn_orient_matrix_UB_31      -0.1305107000
_diffrn_orient_matrix_UB_32      -0.0687955000
_diffrn_orient_matrix_UB_33      -0.0161180000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47311
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.77
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.977
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.5342
_exptl_crystal_size_mid          0.2676
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         12805
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0528P)^2^+5.7913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                11965
_reflns_number_total             12805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501720h_si_002.cif
_cod_data_source_block           neal1n
_cod_original_cell_volume        3221.94(14)
_cod_database_code               4341476
_chemical_oxdiff_formula         'Cu3 S I P6 N3 C72 H63'
_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) groups
2. Shared sites
{I1, S1A}
{S1, I1A}
3. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(S1A)
Uanis(S1) = Uanis(I1A)
4. Same fragment restrains
{I1, Cu1, Cu2, Cu3, S1}
as
{I1A, Cu1A, Cu2A, Cu3A, S1A}
5. Others
 Sof(I1A)=Sof(Cu1A)=Sof(Cu2A)=Sof(Cu3A)=Sof(S1A)=1-FVAR(1)
 Sof(I1)=Sof(Cu1)=Sof(Cu2)=Sof(Cu3)=Sof(S1)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;