Thermochromic Solid-State Emission of Dipyridyl Sulfoxide Cu(I) Complexes
Brown, Christopher M.; Carta, Veronica; Wolf, Michael O.; Chemistry of Materials 30 (2018) 5786–; doi:10.1021/acs.chemmater.8b02821

data_4003128
_publ_section_title
;
 Thermochromic Solid-State Emission of Dipyridyl Sulfoxide Cu(I) Complexes
;
_journal_issue                   16
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5786
_journal_paper_doi               10.1021/acs.chemmater.8b02821
_journal_volume                  30
_journal_year                    2018
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C46 H36 Cu N2 O2 P2 S), 2(B F4)'
_chemical_formula_sum            'C92 H72 B2 Cu2 F8 N4 O4 P4 S2'
_chemical_formula_weight         1786.34
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                101.9908(16)
_cell_angle_beta                 99.5004(16)
_cell_angle_gamma                99.8941(15)
_cell_formula_units_Z            2
_cell_length_a                   10.2401(7)
_cell_length_b                   19.7604(14)
_cell_length_c                   21.4189(15)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.45
_cell_volume                     4084.8(5)
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36823
_diffrn_reflns_theta_full        26.999
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         0.994
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.03
_refine_diff_density_min         -1.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         18675
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.0020159
_refine_ls_shift/su_mean         0.0000381
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.05 5.66 2.47 0.632 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1013
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1013
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                14733
_reflns_number_total             18738
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.64
_oxford_diffrn_Wilson_scale      104.44
_oxford_refine_ls_r_factor_ref   0.0548
_oxford_refine_ls_scale          0.107216(18)
_oxford_reflns_number_all        18676
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DIST 1.43, 0.005 = B(110) TO F(113), B(110) TO F(111) 
CONT  F(109) TO B(110), B(110) TO F(112) 
CONT  B(110) TO F(123), B(110) TO F(121) 
CONT  B(110) TO F(122) 
ANGL 109, 1 = F(109) TO B(110) TO F(112) 
CONT F(109) TO B(110) TO F(111) 
CONT F(109) TO B(110) TO F(113) 
CONT F(112) TO B(110) TO F(113) 
CONT F(112) TO B(110) TO F(111) 
CONT F(113) TO B(110) TO F(111) 
CONT F(109) TO B(110) TO F(121) 
CONT F(109) TO B(110) TO F(123) 
CONT F(122) TO B(110) TO F(123) 
CONT F(122) TO B(110) TO F(121) 
CONT F(123) TO B(110) TO F(121) 
DIST 1.43, 0.005 = B(115) TO F(114), B(115) TO F(116) 
CONT  F(117) TO B(115), B(115) TO F(118) 
CONT  B(115) TO F(124), B(115) TO F(126) 
CONT  B(115) TO F(128) 
ANGL 109, 1 = F(117) TO B(115) TO F(118) 
CONT F(117) TO B(115) TO F(116) 
CONT F(117) TO B(115) TO F(114) 
CONT F(118) TO B(115) TO F(114) 
CONT F(118) TO B(115) TO F(116) 
CONT F(114) TO B(115) TO F(116) 
CONT F(117) TO B(115) TO F(126) 
CONT F(117) TO B(115) TO F(124) 
CONT F(128) TO B(115) TO F(124) 
CONT F(128) TO B(115) TO F(126) 
CONT F(124) TO B(115) TO F(126) 
VIBRATION 0.0, 0.01000 = F(118) TO F(128) 
U(IJ)'S  0.0, 0.005000 = F(118) TO F(128) 
VIBRATION 0.0, 0.01000 = F(114) TO F(124) 
U(IJ)'S  0.0, 0.00500 = F(114) TO F(124) 
VIBRATION 0.0, 0.01000 = F(116) TO F(126) 
U(IJ)'S  0.0, 0.005000 = F(116) TO F(126) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = CU(1) TO N(41) 
VIBR .0, 0.00200 = CU(1) TO S(47) 
VIBR .0, 0.00200 = CU(1) TO N(50) 
VIBR .0, 0.00500 = N(41) TO P(2) 
VIBR .0, 0.00500 = N(41) TO P(28) 
VIBR .0, 0.00500 = S(47) TO P(2) 
VIBR .0, 0.00500 = S(47) TO P(28) 
VIBR .0, 0.00500 = S(47) TO N(41) 
VIBR .0, 0.00500 = N(50) TO P(2) 
VIBR .0, 0.00500 = N(50) TO P(28) 
VIBR .0, 0.00500 = N(50) TO N(41) 
VIBR .0, 0.00500 = N(50) TO S(47) 
VIBR .0, 0.00200 = N(41) TO C(42) 
VIBR .0, 0.00200 = N(41) TO C(46) 
VIBR .0, 0.00500 = C(42) TO CU(1) 
VIBR .0, 0.00500 = C(46) TO CU(1) 
VIBR .0, 0.00500 = C(46) TO C(42) 
VIBR .0, 0.00200 = C(42) TO C(43) 
VIBR .0, 0.00500 = C(43) TO N(41) 
VIBR .0, 0.00200 = C(43) TO C(44) 
VIBR .0, 0.00500 = C(44) TO C(42) 
VIBR .0, 0.00200 = C(44) TO C(45) 
VIBR .0, 0.00500 = C(45) TO C(43) 
VIBR .0, 0.00200 = C(45) TO C(46) 
VIBR .0, 0.00500 = C(46) TO C(44) 
VIBR .0, 0.00200 = C(46) TO S(47) 
VIBR .0, 0.00500 = N(41) TO C(45) 
VIBR .0, 0.00500 = S(47) TO C(45) 
VIBR .0, 0.00500 = S(47) TO N(41) 
VIBR .0, 0.00100 = S(47) TO O(48) 
VIBR .0, 0.00200 = S(47) TO C(49) 
VIBR .0, 0.00500 = CU(1) TO C(46) 
VIBR .0, 0.00250 = O(48) TO C(46) 
VIBR .0, 0.00250 = O(48) TO CU(1) 
VIBR .0, 0.00500 = C(49) TO C(46) 
VIBR .0, 0.00500 = C(49) TO CU(1) 
VIBR .0, 0.00250 = C(49) TO O(48) 
VIBR .0, 0.00200 = C(49) TO N(50) 
VIBR .0, 0.00200 = C(49) TO C(54) 
VIBR .0, 0.00500 = N(50) TO S(47) 
VIBR .0, 0.00500 = C(54) TO S(47) 
VIBR .0, 0.00500 = C(54) TO N(50) 
VIBR .0, 0.00200 = N(50) TO C(51) 
VIBR .0, 0.00500 = CU(1) TO C(49) 
VIBR .0, 0.00500 = C(51) TO C(49) 
VIBR .0, 0.00500 = C(51) TO CU(1) 
VIBR .0, 0.00200 = C(51) TO C(52) 
VIBR .0, 0.00500 = C(52) TO N(50) 
VIBR .0, 0.00100 = C(52) TO C(53) 
VIBR .0, 0.00250 = C(53) TO C(51) 
VIBR .0, 0.00100 = C(53) TO C(54) 
VIBR .0, 0.00500 = C(54) TO C(52) 
VIBR .0, 0.00250 = C(53) TO C(49) 
VIBR .0, 0.00200 = F(109) TO B(110) 
VIBR .0, 0.00200 = B(110) TO F(111) 
VIBR .0, 0.00200 = B(110) TO F(112) 
VIBR .0, 0.00200 = B(110) TO F(113) 
VIBR .0, 0.00500 = F(111) TO F(109) 
VIBR .0, 0.00500 = F(112) TO F(109) 
VIBR .0, 0.00500 = F(112) TO F(111) 
VIBR .0, 0.00500 = F(113) TO F(109) 
VIBR .0, 0.00500 = F(113) TO F(111) 
VIBR .0, 0.00500 = F(113) TO F(112) 
VIBR .0, 0.00200 = F(114) TO B(115) 
VIBR .0, 0.00200 = B(115) TO F(116) 
VIBR .0, 0.00200 = B(115) TO F(117) 
VIBR .0, 0.00200 = B(115) TO F(118) 
VIBR .0, 0.00500 = F(116) TO F(114) 
VIBR .0, 0.00500 = F(117) TO F(114) 
VIBR .0, 0.00500 = F(117) TO F(116) 
VIBR .0, 0.00500 = F(118) TO F(114) 
VIBR .0, 0.00500 = F(118) TO F(116) 
VIBR .0, 0.00500 = F(118) TO F(117) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = CU(1) TO N(41) 
U(IJ) .0, 0.04000 = CU(1) TO S(47) 
U(IJ) .0, 0.04000 = CU(1) TO N(50) 
U(IJ) .0, 0.04000 = N(41) TO C(42) 
U(IJ) .0, 0.04000 = N(41) TO C(46) 
U(IJ) .0, 0.04000 = C(42) TO C(43) 
U(IJ) .0, 0.04000 = C(43) TO C(44) 
U(IJ) .0, 0.04000 = C(44) TO C(45) 
U(IJ) .0, 0.04000 = C(45) TO C(46) 
U(IJ) .0, 0.04000 = C(46) TO S(47) 
U(IJ) .0, 0.02000 = S(47) TO O(48) 
U(IJ) .0, 0.04000 = S(47) TO C(49) 
U(IJ) .0, 0.04000 = C(49) TO N(50) 
U(IJ) .0, 0.04000 = C(49) TO C(54) 
U(IJ) .0, 0.04000 = N(50) TO C(51) 
U(IJ) .0, 0.04000 = C(51) TO C(52) 
U(IJ) .0, 0.02000 = C(52) TO C(53) 
U(IJ) .0, 0.04000 = C(53) TO C(54) 
U(IJ) .0, 0.08000 = F(109) TO B(110) 
U(IJ) .0, 0.08000 = B(110) TO F(111) 
U(IJ) .0, 0.08000 = B(110) TO F(112) 
U(IJ) .0, 0.08000 = B(110) TO F(113) 
U(IJ) .0, 0.08000 = F(114) TO B(115) 
U(IJ) .0, 0.08000 = B(115) TO F(116) 
U(IJ) .0, 0.08000 = B(115) TO F(117) 
U(IJ) .0, 0.08000 = B(115) TO F(118) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBRATION 0.0, 0.010000 = F(112) TO F(122) 
U(IJ)'S  0.0, 0.005000 = F(112) TO F(122) 
VIBRATION 0.0, 0.010000 = F(113) TO F(123) 
U(IJ)'S  0.0, 0.005000 = F(113) TO F(123) 
VIBRATION 0.0, 0.010000 = F(111) TO F(121) 
U(IJ)'S  0.0, 0.005000 = F(111) TO F(121) 
VIBRATION 0.0, 0.010000 = C(33) TO C(34) 
U(IJ)'S  0.0, 0.005000 = C(33) TO C(34) 
END                                                                             
;
_cod_data_source_file            cm8b02821_si_001.cif
_cod_data_source_block           Cu-DPSO
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4003128