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_4341473
_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 N3 P6 S1'
_chemical_formula_sum            'C72 H63 Cu3 N3 P6 S'
_chemical_formula_weight         1378.75
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   22.6945(7)
_cell_length_b                   22.6945(7)
_cell_length_c                   9.9881(5)
_cell_measurement_reflns_used    7276
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.5900
_cell_measurement_theta_min      4.4000
_cell_volume                     4455.1(3)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9815
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0207585000
_diffrn_orient_matrix_UB_12      -0.0753975000
_diffrn_orient_matrix_UB_13      -0.0167932000
_diffrn_orient_matrix_UB_21      0.0742727000
_diffrn_orient_matrix_UB_22      0.0179814000
_diffrn_orient_matrix_UB_23      0.0239349000
_diffrn_orient_matrix_UB_31      -0.0140128000
_diffrn_orient_matrix_UB_32      -0.0115033000
_diffrn_orient_matrix_UB_33      0.1513397000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28120
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.61
_diffrn_reflns_theta_min         3.90
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.470
_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
;
;
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          0.7300
_exptl_crystal_size_mid          0.0498
_exptl_crystal_size_min          0.0379
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5901
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0773
_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^)+(0.1192P)^2^+5.3986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2178
_refine_ls_wR_factor_ref         0.2253
_reflns_number_gt                4785
_reflns_number_total             5901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501720h_si_002.cif
_cod_data_source_block           neal1f
_cod_database_code               4341473
_chemical_oxdiff_formula         'Cu3 S P6 C72 H63 N3'
_reflns_odcompleteness_completeness 99.96
_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 N(H) groups
2. Restrained planarity
 C11A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.1
 C11B, C12B, C13B, C14B, C15B, C16B
 with sigma of 0.1
 C21A, C22A, C23A, C24A, C25A, C26A
 with sigma of 0.1
 C21B, C22B, C23B, C24B, C25B, C26B
 with sigma of 0.1
 C31A, C32A, C33A, C34A, C35A, C36A
 with sigma of 0.1
 C31B, C32B, C33B, C34B, C35B, C36B
 with sigma of 0.1
3. Rigid bond restraints
 C11A, C12A, C13A, C14A, C15A, C16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11B, C12B, C13B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21B, C22B, C23B, C24B, C25B, C26B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31A, C32A, C33A, C34A, C35A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31B, C32B, C33B, C34B, C35B, C36B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C11B) = Uanis(C11A)
Uanis(C12B) = Uanis(C12A)
Uanis(C13B) = Uanis(C13A)
Uanis(C21A) = Uanis(C21B)
Uanis(C31A) = Uanis(C31B)
Uanis(C35A) = Uanis(C35B)
Uanis(C36A) = Uanis(C36B)
Uanis(C25A) = Uanis(C25B)
Uanis(C26A) = Uanis(C26B)
Uanis(C23A) = Uanis(C23B)
Uanis(C22A) = Uanis(C22B)
Uanis(C24A) = Uanis(C24B)
Uanis(C14B) = Uanis(C14A)
Uanis(C15A) = Uanis(C15B)
Uanis(C16A) = Uanis(C16B)
Uanis(C33B) = Uanis(C33A)
Uanis(C34B) = Uanis(C34A)
Uanis(C32A) = Uanis(C32B)
5. Same fragment restrains
{C11A, C12A, C13A, C14A, C15A, C16A}
as
{C11B, C12B, C13B, C14B, C15B, C16B}
{C11A, C12A, C13A, C14A, C15A, C16A}
as
{C21A, C22A, C23A, C24A, C25A, C26A}
{C11A, C12A, C13A, C14A, C15A, C16A}
as
{C21B, C22B, C23B, C24B, C25B, C26B}
{C11A, C12A, C13A, C14A, C15A, C16A}
as
{C31A, C32A, C33A, C34A, C35A, C36A}
{C11A, C12A, C13A, C14A, C15A, C16A}
as
{C31B, C32B, C33B, C34B, C35B, C36B}
6. Others
 Fixed Sof: C11A(0.66667) C12A(0.66667) H12A(0.66667) C13A(0.66667)
 H13A(0.66667) C14A(0.66667) H14A(0.66667) C15A(0.66667) H15A(0.66667)
 C16A(0.66667) H16A(0.66667) C11B(0.33333) C12B(0.33333) H12B(0.33333)
 C13B(0.33333) H13B(0.33333) C14B(0.33333) H14B(0.33333) C15B(0.33333)
 H15B(0.33333) C16B(0.33333) H16B(0.33333) C21A(0.66667) C22A(0.66667)
 H22A(0.66667) C23A(0.66667) H23A(0.66667) C24A(0.66667) H24A(0.66667)
 C25A(0.66667) H25A(0.66667) C26A(0.66667) H26A(0.66667) C21B(0.33333)
 C22B(0.33333) H22B(0.33333) C23B(0.33333) H23B(0.33333) C24B(0.33333)
 H24B(0.33333) C25B(0.33333) H25B(0.33333) C26B(0.33333) H26B(0.33333)
 C31A(0.66667) C32A(0.66667) H32A(0.66667) C33A(0.66667) H33A(0.66667)
 C34A(0.66667) H34A(0.66667) C35A(0.66667) H35A(0.66667) C36A(0.66667)
 H36A(0.66667) C31B(0.33333) C32B(0.33333) H32B(0.33333) C33B(0.33333)
 H33B(0.33333) C34B(0.33333) H34B(0.33333) C35B(0.33333) H35B(0.33333)
 C36B(0.33333) H36B(0.33333)
7.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A),
 C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C22A(H22A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C22B(H22B), C23B(H23B),
 C24B(H24B), C25B(H25B), C26B(H26B), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B),
 C36B(H36B), C46(H46), C45(H45), C42(H42), C44(H44), C43(H43)
;