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_7711113
_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 H12 La N7 O9, H2 O'
_chemical_formula_sum            'C6 H14 La N7 O10'
_chemical_formula_weight         483.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           24
_space_group_name_Hall           'I 2b 2c'
_space_group_name_H-M_alt        'I 21 21 21'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5379(2)
_cell_length_b                   10.6082(3)
_cell_length_c                   19.3914(6)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100
_cell_measurement_theta_max      54.953
_cell_measurement_theta_min      3.968
_cell_volume                     1344.90(7)
_computing_cell_refinement
;
SAINT (2013) V8.37A; 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) V8.37A; 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 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11309
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.927
_diffrn_reflns_theta_min         3.967
_exptl_absorpt_coefficient_mu    17.378
_exptl_absorpt_correction_T_max  0.0766
_exptl_absorpt_correction_T_min  0.0125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1237 before and 0.0415 after correction.
The Ratio of minimum to maximum transmission is 0.1632.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light Colorless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    2.386
_exptl_crystal_description       Block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.417(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1271
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.350
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0667P)^2^+0.6704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.690
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1269
_reflns_number_total             1271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01924h2.cif
_cod_data_source_block           la-cy
_cod_database_code               7711113
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.304
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.583(14)
 0.417(14)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H,H,H,H,H,H,H) groups
3. Restrained distances
 O4-H4A = O4-H4B = O3-H3A = O3-H3B = O5-H5A = O5-H5B = O6-H6A = O6-H6B
 0.85 with sigma of 0.002
 H4A-H4B = H3A-H3B = H5A-H5B = H6A-H6B
 1.3 with sigma of 0.002
 H4A-H3B_$3
 2.2 with sigma of 0.02
 H6A-H6A_$6
 2.2 with sigma of 0.02
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5)
5.a Rotating group:
 N4(O4,O3,O2,O5,O6,H4A,H4B), O6(H6A,H6B), O6(H5A,H5B), O6(H3A,H3B)
;
_shelx_res_checksum              51367
_shelx_hkl_checksum              30728
_olex2_submission_special_instructions 'No special instructions were received'