Syntheses, structures, and luminescence of a series of novel trimetallic coordination polymers constructed by Cu-I clusters and alkaline-carboxyl- alkaline-earth building units
Xiong, Gang; Wang, Bin-bin; He, Yongke; you, Lixin; Ren, Baoyi; Sun, Yaguang; Journal of Solid State Chemistry 265 (2018) 393–401; doi:10.1016/j.jssc.2018.06.026

data_1561022
_publ_section_title
;
 Syntheses, structures, and luminescence of a series of novel trimetallic
 coordination polymers constructed by Cu-I clusters and alkaline-carboxyl-
 alkaline-earth building units
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              393
_journal_page_last               401
_journal_paper_doi               10.1016/j.jssc.2018.06.026
_journal_volume                  265
_journal_year                    2018
_chemical_formula_moiety         'C42 H29 Ba2 Cu2 I Li2 N7 O15.5'
_chemical_formula_sum            'C42 H29 Ba2 Cu2 I Li2 N7 O15.5'
_chemical_formula_weight         1422.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.392(6)
_cell_length_b                   27.158(11)
_cell_length_c                   28.376(11)
_cell_measurement_reflns_used    20957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.009
_cell_measurement_theta_min      3.015
_cell_volume                     11091(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1392
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            78766
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.015
_exptl_absorpt_coefficient_mu    2.780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL shelx in Pbca #61
CELL   14.3920   27.1580   28.3760     90.00     90.00     90.00
SPGR Pbca
Q101 0.598 0.712 0.842 !       1.63 eA-3
C102 0.193 0.189 0.268 !       1.59 eA-3
C103 0.500 0.805 0.672 !       1.55 eA-3
Q104 0.295 0.196 0.251 !       1.55 eA-3
Q105 0.989 0.205 0.212 !       1.52 eA-3
C106 0.221 0.210 0.264 !       1.49 eA-3
C107 0.649 0.672 0.216 !       1.49 eA-3
Q108 0.018 0.993 0.839 !       1.47 eA-3
C109 0.969 0.736 0.318 !       1.38 eA-3
C110 0.440 0.728 0.730 !       1.36 eA-3
Q111 0.267 0.779 0.030 !       1.33 eA-3
C112 0.559 0.654 0.191 !       1.29 eA-3
Q113 0.527 0.297 0.516 !       1.29 eA-3
Q114 0.011 0.695 0.256 !       1.29 eA-3
Q115 0.235 0.241 0.149 !       1.28 eA-3
C116 0.496 0.871 0.724 !       1.27 eA-3
C117 0.769 0.735 0.262 !       1.26 eA-3
C118 0.484 0.337 0.249 !       1.25 eA-3
C119 0.712 0.688 0.209 !       1.24 eA-3
Q120 0.878 0.986 0.790 !       1.24 eA-3
Q121 0.888 0.094 0.162 !       1.24 eA-3
Q122 0.129 0.246 0.186 !       1.22 eA-3
Q123 0.985 0.470 0.697 !       1.22 eA-3
C124 0.060 0.219 0.196 !       1.20 eA-3
C125 0.988 0.616 0.305 !       1.20 eA-3
Q126 0.671 0.415 0.399 !       1.20 eA-3
Q127 0.766 0.767 0.694 !       1.19 eA-3
Q128 0.019 0.497 0.250 !       1.19 eA-3
Q129 0.589 0.658 0.221 !       1.19 eA-3
Q130 0.436 0.234 0.371 !       1.18 eA-3
C131 0.248 0.173 0.290 !       1.17 eA-3
Q132 0.861 0.358 0.216 !       1.16 eA-3
Q133 0.495 0.165 0.079 !       1.16 eA-3
Q134 0.530 0.347 0.749 !       1.15 eA-3
Q135 0.288 0.147 0.673 !       1.15 eA-3
Q136 0.713 0.223 0.827 !       1.14 eA-3
Q137 1.000 0.165 0.378 !       1.14 eA-3
Q138 0.988 0.830 0.742 !       1.14 eA-3
Q139 0.020 0.263 0.763 !       1.13 eA-3
Q140 0.236 0.110 0.209 !       1.13 eA-3
Q141 0.793 0.222 0.181 !       1.12 eA-3
Q142 0.508 0.482 0.939 !       1.12 eA-3
Q143 0.969 0.240 0.763 !       1.11 eA-3
Q144 0.612 0.720 0.209 !       1.11 eA-3
Q145 0.301 0.217 0.220 !       1.11 eA-3
Q146 0.699 0.783 0.780 !       1.11 eA-3
Q147 0.544 0.854 0.735 !       1.11 eA-3
Q148 0.520 0.322 0.289 !       1.10 eA-3
Q149 0.877 0.271 0.807 !       1.10 eA-3
C150 0.014 0.649 0.302 !       1.10 eA-3
C151 0.427 0.213 0.314 !       1.10 eA-3
Q152 0.727 0.241 0.422 !       1.10 eA-3
Q153 0.194 0.353 0.804 !       1.09 eA-3
Q154 0.049 0.692 0.767 !       1.09 eA-3
C155 0.891 0.805 0.812 !       1.09 eA-3
Q156 0.202 0.431 0.217 !       1.09 eA-3
Q157 0.531 0.671 0.967 !       1.09 eA-3
Q158 0.541 0.492 0.718 !       1.08 eA-3
Q159 0.112 0.213 0.633 !       1.08 eA-3
C160 0.701 0.839 0.689 !       1.08 eA-3
Q161 0.780 0.260 0.545 !       1.08 eA-3
Q162 0.906 0.789 0.220 !       1.07 eA-3
Q163 0.551 0.227 0.938 !       1.07 eA-3
C164 0.895 0.663 0.268 !       1.07 eA-3
Q165 0.079 0.800 0.205 !       1.07 eA-3
C166 0.616 0.821 0.706 !       1.07 eA-3
Q167 0.536 0.834 0.125 !       1.07 eA-3
Q168 0.812 0.750 0.287 !       1.06 eA-3
Q169 1.000 0.210 0.702 !       1.06 eA-3
Q170 0.265 0.260 0.478 !       1.05 eA-3
Q171 0.579 0.716 0.261 !       1.05 eA-3
Q172 0.112 0.125 0.246 !       1.04 eA-3
Q173 0.575 0.211 0.267 !       1.04 eA-3
Q174 0.142 0.763 0.876 !       1.04 eA-3
Q175 0.144 0.618 0.694 !       1.04 eA-3
Q176 0.594 0.284 0.254 !       1.04 eA-3
Q177 0.652 0.712 0.841 !       1.03 eA-3
C178 0.789 0.720 0.303 !       1.03 eA-3
C179 0.118 0.876 0.793 !       1.03 eA-3
Q180 0.574 0.477 0.353 !       1.03 eA-3
Q181 0.566 0.029 0.297 !       1.03 eA-3
Q182 0.605 0.547 0.713 !       1.02 eA-3
Q183 0.373 0.973 0.650 !       1.02 eA-3
C184 0.107 0.634 0.266 !       1.02 eA-3
Q185 0.886 0.720 0.795 !       1.02 eA-3
Q186 0.014 0.997 0.668 !       1.02 eA-3
Q187 0.816 0.200 0.756 !       1.01 eA-3
Q188 0.559 0.316 0.689 !       1.01 eA-3
Q189 0.320 0.501 0.702 !       1.01 eA-3
Q190 0.611 0.256 0.561 !       1.01 eA-3
Q191 0.156 0.878 0.827 !       1.01 eA-3
Q192 0.468 0.857 0.142 !       1.01 eA-3
Q193 0.060 0.117 0.514 !       1.00 eA-3
Q194 0.183 0.210 0.495 !       1.00 eA-3
Q195 0.059 0.449 0.029 !       1.00 eA-3
C196 0.341 0.724 0.227 !       1.00 eA-3
Q197 0.178 0.493 0.288 !       1.00 eA-3
Q198 0.795 0.745 0.561 !       0.99 eA-3
Q199 0.359 0.866 0.276 !       0.99 eA-3
;
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+50.6949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7572
_reflns_number_total             9718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            7.cif
_cod_data_source_block           shelx_sq
_cod_original_formula_sum        'C42 H29 Ba2 Cu2 I Li2 N7 O15.50'
_cod_database_code               1561022
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C33-C37
 1.53 with sigma of 0.01
 H15B-Ba1
 3 with sigma of 0.01
 H38_$1-H15A_$2
 2.1 with sigma of 0.01
 H15A-O15
 0.85 with sigma of 0.01
 O15-H15B
 0.85 with sigma of 0.01
 H15A-H15B
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Li2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ba1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) = Uanis(O17)
4. Others
 Fixed Sof: O15(0.5) H15A(0.5) H15B(0.5) O16(0.5) O17(0.5)
5.a Fixed occupancy and ADP/Uiso:
 H15B
5.b Riding coordinates:
 O15(H15A)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C27(H27), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C41(H41), C42(H42)
5.d Fitted hexagon refined as free rotating group:
 N7(C38,C39,C40,C41,C42)
;
_platon_squeeze_void_probe_radius 1.20
_cod_database_fobs_code 1561022