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_4350659
_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         'C46 H49 Cu2 I2 N O8 P2'
_chemical_formula_sum            'C46 H49 Cu2 I2 N O8 P2'
_chemical_formula_weight         1186.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-01-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.059(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5661(8)
_cell_length_b                   15.8160(6)
_cell_length_c                   18.4637(9)
_cell_measurement_temperature    150.15
_cell_volume                     4836.8(4)
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.900
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53245
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        31.000
_diffrn_reflns_theta_max         32.912
_diffrn_reflns_theta_min         2.971
_exptl_absorpt_coefficient_mu    2.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            '? colourless'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.900
_refine_diff_density_min         -3.671
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         16295
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1372P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2211
_refine_ls_wR_factor_ref         0.2366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10940
_reflns_number_total             16295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500240j_si_001.cif
_cod_data_source_block           msb047a
_cod_database_code               4350659
_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
 C15-C18 = C15-C18A = C31-C34 = C31-C34A = C41-C44 = C41-C44A
 1.523 with sigma of 0.003
 C18-C19 = C18A-C19A = C34-C35 = C34A-C35A = C44-C45 = C44A-C45A
 1.504 with sigma of 0.004
 C19-C20 = C19A-C20A = C35-C36 = C35A-C36A = C45-C46 = C45A-C46A
 1.295 with sigma of 0.005
 C15-C19 = C15-C19A = C31-C35 = C31-C35A = C41-C45 = C41-C45A
 2.513 with sigma of 0.006
 C18-C20 = C18A-C20A = C34-C36 = C34A-C36A = C44-C46 = C44A-C46A
 2.467 with sigma of 0.007
3. Uiso/Uaniso restraints and constraints
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(C45A) \\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
Uanis(C36) = Uanis(C36A)
Uanis(C44) = Uanis(C44A)
Uanis(C45) = Uanis(C45A)
Uanis(C46) = Uanis(C46A)
4. Others
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 FVAR(1)
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36C)=
 Sof(H36D)=1-FVAR(2)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 FVAR(2)
 Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46C)=
 Sof(H46D)=1-FVAR(3)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), 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), 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), C45A(H45A)
5.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), 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   0.741
_shelx_estimated_absorpt_t_min   0.623
_shelxl_version_number           2012-9