Short-bite PNP ligand-supported rare tetranuclear [Cu4I4] clusters: structural and photoluminescence studies.
Naik, Susmita; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic chemistry 53 (2014) 3864–3873; doi:10.1021/ic500240j

data_4350657
_publ_section_title
;
 Short-bite PNP ligand-supported rare tetranuclear [Cu4I4] clusters:
 structural and photoluminescence studies.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3864
_journal_page_last               3873
_journal_paper_doi               10.1021/ic500240j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C92 H98 Cl4 Cu4 N2 O16 P4'
_chemical_formula_sum            'C92 H98 Cl4 Cu4 N2 O16 P4'
_chemical_formula_weight         2007.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-12-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                111.404(2)
_cell_angle_beta                 92.821(2)
_cell_angle_gamma                100.448(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8854(3)
_cell_length_b                   14.2961(4)
_cell_length_c                   15.0486(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2322.49(11)
_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  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.871
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29612
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.852
_diffrn_reflns_theta_min         3.134
_exptl_absorpt_coefficient_mu    1.152
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         15042
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0601P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10114
_reflns_number_total             15042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500240j_si_001.cif
_cod_data_source_block           msb048
_cod_database_code               4350657
_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. Restrained distances
 C8-C9 = C8A-C9A = C18-C19 = C18A-C19A = C34-C35 = C34A-C35A
 1.504 with sigma of 0.003
 C9-C10 = C9A-C10A = C19-C20 = C19A-C20A = C35-C36 = C35A-C36A
 1.304 with sigma of 0.004
 C8-C10 = C8A-C10A = C18-C20 = C18A-C20A = C34-C36 = C34A-C36A
 2.467 with sigma of 0.006
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq, 
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C45B) \\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
Uanis(C46) = Uanis(C46A)
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C34) = Uanis(C34A)
Uanis(C20) = Uanis(C20A)
Uanis(C19) = Uanis(C19A)
Uanis(C18) = Uanis(C18A)
Uanis(C10) = Uanis(C10A)
Uanis(C9) = Uanis(C9A)
Uanis(C8) = Uanis(C8A)
4. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=
 1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 FVAR(2)
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36C)=
 Sof(H36D)=1-FVAR(3)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 FVAR(3)
 Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45B)=Sof(C46A)=Sof(H46C)=
 Sof(H46D)=1-FVAR(4)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C8A(H8AA,H8AB), C18(H18A,H18B), C18A(H18C,H18D), C34(H34A,H34B),
 C34A(H34C,H34D), C44(H44A,H44B), C44A(H44C,H44D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C9(H9), C9A(H9A), C14(H14), C16(H16), C17(H17),
 C19(H19), C19A(H19A), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C30(H30), C32(H32), C33(H33), C35(H35), C35A(H35A), C40(H40), C42(H42),
 C43(H43), C45(H45), C45B(H45B)
5.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C10A(H10C,H10D), C20(H20A,H20B), C20A(H20C,H20D), C36(H36A,
 H36B), C36A(H36C,H36D), C46(H46A,H46B), C46A(H46C,H46D)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C)
;
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.709
_shelx_hkl_checksum              17440
_shelx_res_checksum              33341
_shelxl_version_number           2012-9