Luminescence Solvato- and Vapochromism of Alkynyl-Phosphine Copper Clusters.
Krytchankou, Ilya S.; Koshevoy, Igor O.; Gurzhiy, Vladislav V.; Pomogaev, Vladimir A.; Tunik, Sergey P.; Inorganic chemistry 54 (2015) 8288–8297; doi:10.1021/acs.inorgchem.5b00239

data_4346072
_publ_section_title
;
 Luminescence Solvato- and Vapochromism of Alkynyl-Phosphine Copper
 Clusters.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8288
_journal_page_last               8297
_journal_paper_doi               10.1021/acs.inorgchem.5b00239
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C57 H48 Cu3 N O2 P3), 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C118 H102 Cu6 F12 N4 O4 P8'
_chemical_formula_weight         2497.03
_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             2014-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-09-17 # Formatted by publCIF
;
_cell_angle_alpha                88.5779(10)
_cell_angle_beta                 81.0200(11)
_cell_angle_gamma                78.5399(13)
_cell_formula_units_Z            2
_cell_length_a                   12.7133(2)
_cell_length_b                   17.8070(3)
_cell_length_c                   24.1678(2)
_cell_measurement_reflns_used    61575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1030
_cell_measurement_theta_min      3.7830
_cell_volume                     5296.33(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0072628000
_diffrn_orient_matrix_UB_12      0.0841735000
_diffrn_orient_matrix_UB_13      -0.0181874000
_diffrn_orient_matrix_UB_21      -0.0543467000
_diffrn_orient_matrix_UB_22      0.0265763000
_diffrn_orient_matrix_UB_23      0.0596619000
_diffrn_orient_matrix_UB_31      0.1124898000
_diffrn_orient_matrix_UB_32      -0.0011004000
_diffrn_orient_matrix_UB_33      0.0165733000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1283
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            175451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.996
_diffrn_reflns_theta_min         3.127
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent colorless'
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1372
_refine_ls_number_reflns         20061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+22.9979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16955
_reflns_number_total             20061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00239_si_003.cif
_cod_data_source_block           2b
_cod_original_cell_volume        5296.31(13)
_cod_database_code               4346072
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 94.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F3'A) = Uanis(F5'A) = Uanis(F4'A) = Uanis(F2'B) = Uanis(F6'B) =
Uanis(F3'B) = Uanis(F1'A) = Uanis(F1'B) = Uanis(F4'B) = Uanis(F2'A) =
Uanis(F6'A) = Uanis(F5'B)
Uanis(F6A) = Uanis(F1A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4A) = Uanis(F5A) =
Uanis(F6A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4B) = Uanis(F2B) = Uanis(F6B)
3. Others
 Sof(F6'B)=Sof(F5'B)=Sof(F2'B)=Sof(F4'B)=Sof(F3'B)=Sof(F1'B)=1-FVAR(1)
 Sof(F1'A)=Sof(F2'A)=Sof(F3'A)=Sof(F4'A)=Sof(F5'A)=Sof(F6'A)=FVAR(1)
 Fixed Sof: F1A(0.5) F2A(0.5) F3A(0.5) F4A(0.5) F5A(0.5) F6A(0.5) F1B(0.5)
 F5B(0.5) F3B(0.5) F4B(0.5) F2B(0.5) F6B(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C1'(H1')
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C5'(H5'), C6'(H6'), C8'(H8'), C9'(H9'), C13'(H13'), C14'(H14'), C16'(H16'),
 C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'), C23'(H23'),
 C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29'), C31'(H31'),
 C32'(H32'), C33'(H33'), C34'(H34'), C35'(H35'), C37'(H37'), C38'(H38'),
 C39'(H39'), C40'(H40'), C41'(H41'), C43'(H43'), C44'(H44'), C45'(H45'),
 C46'(H46'), C47'(H47'), C49'(H49'), C50'(H50'), C51'(H51'), C52'(H52'),
 C53'(H53')
4.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C55'(H55D,H55E,
 H55F), C56'(H56D,H56E,H56F), C57'(H57D,H57E,H57F), C59'(H59A,H59B,H59C),
 C59(H59D,H59E,H59F)
;