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_1561021
_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         'C40 H50 Ba2 Cu2 I2 Li2 N8 O16, 0.5(H2 O)'
_chemical_formula_sum            'C40 H47 Ba2 Cu2 I2 Li2 N8 O16.5'
_chemical_formula_weight         1573.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2bc 2ac'
_space_group_name_H-M_alt        'P c a b'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.363(5)
_cell_length_b                   27.061(8)
_cell_length_c                   26.853(7)
_cell_measurement_reflns_used    22793
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11890(6)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1500
	          2theta: 29.8962
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1500
	          2theta: 29.8962
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1500
	          2theta: 29.8962
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.017287
_diffrn_orient_matrix_UB_12      0.057066
_diffrn_orient_matrix_UB_13      0.013399
_diffrn_orient_matrix_UB_21      0.017392
_diffrn_orient_matrix_UB_22      -0.002367
_diffrn_orient_matrix_UB_23      0.032518
_diffrn_orient_matrix_UB_31      0.031123
_diffrn_orient_matrix_UB_32      0.013112
_diffrn_orient_matrix_UB_33      -0.015691
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            88741
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10460
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0416P)^2^+191.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8243
_reflns_number_total             10460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        11891(6)
_cod_original_formula_sum        'C40 H47 Ba2 Cu2 I2 Li2 N8 O16.50'
_cod_database_code               1561021
_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, All O(H,H) groups
2. Restrained distances
 C41-N5
 1.46 with sigma of 0.01
 C30-C37
 2.7 with sigma of 0.01
 C37-N6
 1.5 with sigma of 0.01
 H38B-H37B
 2.1 with sigma of 0.01
 C30-O16
 1.28 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C35 \\sim C41 \\sim N5 \\sim C33 \\sim O14: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C34 \\sim C36 \\sim N8 \\sim C29 \\sim O15: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C38 \\sim C37 \\sim N6 \\sim C30: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C38 \\sim N6 \\sim C37 \\sim C30 \\sim O16: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C32) = Uanis(C40)
4. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: O17(0.5) H17A(0.5) H17B(0.5)
5.a Free rotating group:
 O17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C41(H41)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_cod_database_fobs_code 1561021