Solvent effect on the structures of three manganese complexes based on azotetrazole-3-hydroxy-2-naphthoic acid: synthesis, structures, and magnetic and fluorescent properties
Zhong, Yun-Jing; Ouyang, Zhi-Jian; Kuang, Xiao-Man; Li, You-Hong; Chen, Wen-Bin; Yang, Meng; Dong, Wen; CrystEngComm 25 (2023) 5524–5532; doi:10.1039/D3CE00678F

data_7247329
_publ_section_title
;
 Solvent effect on the structures of three manganese complexes based on
 azotetrazole-3-hydroxy-2-naphthoic acid: synthesis, structures, and
 magnetic and fluorescent properties
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5524
_journal_page_last               5532
_journal_paper_doi               10.1039/D3CE00678F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C30 H28 Mn3 N14 O10, C3 H7 N O, 2(H2 O)'
_chemical_formula_sum            'C33 H39 Mn3 N15 O13'
_chemical_formula_weight         1018.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7912(13)
_cell_length_b                   20.2706(13)
_cell_length_c                   10.2341(6)
_cell_measurement_reflns_used    4595
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.345
_cell_measurement_theta_min      2.642
_cell_volume                     4405.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17323
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.641
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0710 before and 0.0491 after correction. The Ratio of minimum to maximum transmission is 0.8801. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5011
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1000P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3637
_reflns_number_total             5066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00678f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7247329--7247331.cif.'
_cod_database_code               7247329
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Restrained distances
 O6-C16
 1.24 with sigma of 0.01
 N10-C16
 1.34 with sigma of 0.01
 N10-C17 = N10-C18
 1.48 with sigma of 0.01
 N10-C17 \\sim N10-C18
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N8) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(N5)=Sof(N7)=1-FVAR(1)
 Sof(N6)=Sof(N4)=FVAR(1)
 Fixed Sof: H17A(0.5) H17B(0.5) H17C(0.5) N10(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C16(0.5) H16(0.5) O6(0.5) O7(0.6) H7A(0.6) H7B(0.6) O8(0.4) H8A(0.4)
 H8B(0.4)
4.a Riding coordinates:
 C18(H18A,H18B,H18C)
4.b Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
4.c Rotating group:
 O3(H3A)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C8(H8), C9(H9), C13(H13), C10(H10), C16(H16)
4.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              62963
_olex2_submission_special_instructions 'No special instructions were received'