S-Heptazine N-Ligand Based Luminescent Coordination Materials: Synthesis, Structural and Luminescent Studies of Lanthanide-Cyamelurate Networks
Essalhi, Mohamed; Mohan, Midhun; Marineau-Plante, Gabriel; Schlachter, Adrien Camille; Maris, Thierry; Harvey, Pierre D.; Duong, Adam; Dalton Transactions  (2022) –; doi:10.1039/D2DT01924H

data_7711112
_publ_section_title
;
 S-Heptazine N-Ligand Based Luminescent Coordination Materials: Synthesis,
 Structural and Luminescent Studies of Lanthanide-Cyamelurate Networks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01924H
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H8 Er N7 O7, H2 O'
_chemical_formula_sum            'C6 H10 Er N7 O8'
_chemical_formula_weight         475.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-10 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.69360(10)
_cell_length_b                   12.0266(3)
_cell_length_c                   17.6197(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.708
_cell_measurement_theta_min      2.508
_cell_volume                     1206.36(5)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14564
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.701
_diffrn_reflns_theta_min         5.021
_diffrn_source_current           0.65
_diffrn_source_power             0.029119999999999997
_diffrn_source_voltage           44.8
_exptl_absorpt_coefficient_mu    13.558
_exptl_absorpt_correction_T_max  0.0565
_exptl_absorpt_correction_T_min  0.0027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1000 before and 0.0268 after correction. The Ratio of minimum to maximum transmission is 0.0478. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_recrystallization_method 'crystallized form EtOH'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.543
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.080(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2123
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0477P)^2^+0.4017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                2123
_reflns_number_total             2123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01924h2.cif
_cod_data_source_block           er-cy
_cod_database_code               7711112
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.920(15)
 0.080(15)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H,H,H,H,H,H,H,H,H) groups
3. Restrained distances
 O4-H4A \\sim O4-H4B \\sim O5-H5A \\sim O5-H5B \\sim O7-H7A \\sim O7-H7B \\sim
O8-H8A \\sim O8-H8B
 with sigma of 0.02
 H4A-H4B \\sim H5A-H5B \\sim H7A-H7B \\sim H8A-H8B
 with sigma of 0.02
4.a Rotating group:
 C6(O4,O5,O6,O7,O8,H5A,H5B), O8(H4A,H4B), O8(H8A,H8B), O8(H7A,H7B), O8(H6A,H6B)
;
_shelx_res_checksum              75086
_shelx_hkl_checksum              30068
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'