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_4341474
_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         'C75 H138 Cu3 P6 S, C3 H6 O, F6 P'
_chemical_formula_sum            'C78 H144 Cu3 F6 O P7 S'
_chemical_formula_weight         1651.40
_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             2014-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                83.8839(17)
_cell_angle_beta                 86.2996(15)
_cell_angle_gamma                77.4184(17)
_cell_formula_units_Z            2
_cell_length_a                   14.7920(3)
_cell_length_b                   16.0721(4)
_cell_length_c                   18.7434(4)
_cell_measurement_reflns_used    48404
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6840
_cell_measurement_theta_min      3.6660
_cell_volume                     4320.35(17)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0600590000
_diffrn_orient_matrix_UB_12      0.0535136000
_diffrn_orient_matrix_UB_13      -0.0469232000
_diffrn_orient_matrix_UB_21      -0.0795314000
_diffrn_orient_matrix_UB_22      0.0315655000
_diffrn_orient_matrix_UB_23      -0.0519837000
_diffrn_orient_matrix_UB_31      -0.0384126000
_diffrn_orient_matrix_UB_32      0.0766369000
_diffrn_orient_matrix_UB_33      0.0440622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80468
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.71
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.728
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.672
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.1891
_exptl_crystal_size_mid          0.1305
_exptl_crystal_size_min          0.1121
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         17149
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+2.1667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                15862
_reflns_number_total             17149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501720h_si_002.cif
_cod_data_source_block           neal1k
_cod_original_cell_volume        4320.34(15)
_cod_database_code               4341474
_chemical_oxdiff_formula         'Cu3 S P7 F6 C75 H138'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 C64, C65, C66, C67, C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C64A, C65A, C66A, C67A, C68A, C69A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C65A) = Uanis(C65)
4. Same fragment restrains
{C64, C65, C66, C67, C68, C69}
as
{C64A, C65A, C66A, C67A, C68A, C69A}
5. Others
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=
 Sof(H66D)=Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=
 Sof(C69A)=Sof(H69C)=Sof(H69D)=1-FVAR(1)
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=
 Sof(H69B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C14(H14), C20(H20), C27(H27), C33(H33), C39(H39), C45(H45),
 C52(H52), C59(H59), C64(H64), C64A(H64A), C70(H70)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,
 H58B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
  C65A(H65C,H65D), C66A(H66C,H66D), C67A(H67C,H67D), C68A(H68C,H68D), C69A(H69C,
 H69D), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
 C75(H75A,H75B)
6.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
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