De novo synthesis of hybrid d–f block metal complex salts for electronic charge transport applications
Mahato, Shreya; Mondal, Amit; Das, Mainak; Joshi, Mayank; Ray, Partha Pratim; Roy Choudhury, Angshuman; Reddy, C. Malla; Biswas, Bhaskar; Dalton Transactions  (2022) –; doi:10.1039/D1DT02722K

data_7709243
_publ_section_title
;
 &#x000D; De novo synthesis of hybrid d--f block metal complex salts for
 electronic charge transport applications
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02722K
_journal_year                    2022
_chemical_formula_moiety
'2(C24 H16 Cu N5 O3), H N O3, Ce N4.48 O12.96, 2(N0.76 O2.52)'
_chemical_formula_sum            'C48 H33 Ce Cu2 N17 O27'
_chemical_formula_weight         1547.13
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-11-09 deposited with the CCDC.	2022-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                77.538(8)
_cell_angle_beta                 88.428(8)
_cell_angle_gamma                80.416(8)
_cell_formula_units_Z            1
_cell_length_a                   10.5189(7)
_cell_length_b                   10.9751(4)
_cell_length_c                   12.8796(7)
_cell_measurement_reflns_used    4427
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.9
_cell_volume                     1431.55(14)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_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      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
scan:
	Number of images: 629
	           Slice: -69.0000 - 119.7000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 49.8600
	          2theta: 29.8900
scan:
	Number of images: 629
	           Slice: -69.0000 - 119.7000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 180.0000
	             XTD: 49.8600
	          2theta: 29.8900
scan:
	Number of images: 629
	           Slice: -69.0000 - 119.7000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 90.0000
	             XTD: 49.8600
	          2theta: 29.8900
scan:
	Number of images: 629
	           Slice: -69.0000 - 119.7000
	     Image width: 0.3000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 270.0000
	             XTD: 49.8600
	          2theta: 29.8900
;
_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      0.008070
_diffrn_orient_matrix_UB_12      -0.034316
_diffrn_orient_matrix_UB_13      -0.089741
_diffrn_orient_matrix_UB_21      -0.011081
_diffrn_orient_matrix_UB_22      -0.081430
_diffrn_orient_matrix_UB_23      0.046862
_diffrn_orient_matrix_UB_31      -0.075084
_diffrn_orient_matrix_UB_32      0.021060
_diffrn_orient_matrix_UB_33      -0.015559
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20423
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.769
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessings, 1995'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0760P)^2^+4.6304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6113
_reflns_number_total             6494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02722k2.cif
_cod_data_source_block           cuoacphencan_100k
_cod_database_code               7709243
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Shared sites
{N6A, N6B}
{N7A, N7B}
{N8A, N8B}
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C20)
Uanis(C7) = Uanis(C19)
Uanis(N5) = Uanis(N9)
Uanis(O2) = Uanis(O1)
Uanis(N6A) = Uanis(N6B)
Uanis(N7A) = Uanis(N7B)
Uanis(N8A) = Uanis(N8B)
Uanis(C19) = Uanis(C18)
Uanis(C18) = Uanis(C22)
4. Others
 Sof(O2B)=Sof(O3B)=Sof(O1B)=Sof(O5B)=Sof(O4B)=Sof(O6B)=Sof(N6B)=Sof(N7B)=
 Sof(N8B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N6A)=Sof(N7A)=
 Sof(N8A)=FVAR(1)
 Fixed Sof: O13(0.5) O14(0.5) O15(0.5) H15A(0.5) N9(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
5.b Idealised tetrahedral OH refined as rotating group:
 O15(H15A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'