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_7247331
_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
'2(C24.6 H23.80 Mn3 N12 O12.30 S0.3), 7.4(C2 H6 O S), H0.50'
_chemical_formula_sum            'C64 H93 Mn6 N24 O32.5 S8'
_chemical_formula_weight         2304.75
_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   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                82.3150(10)
_cell_angle_beta                 79.293(2)
_cell_angle_gamma                72.4750(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6758(13)
_cell_length_b                   12.4221(15)
_cell_length_c                   19.041(2)
_cell_measurement_reflns_used    6740
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.250
_cell_measurement_theta_min      2.300
_cell_volume                     2357.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19002
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_min         1.092
_diffrn_source                   '\f and \w scans'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0550 before and 0.0345 after correction. The Ratio of minimum to maximum transmission is 0.8830. The \l/2 correction factor is 0.00150.'
_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    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         10085
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1000P)^2^+19.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8258
_reflns_number_total             10085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00678f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7247329--7247331.cif.'
_cod_original_cell_volume        2357.9(5)
_cod_original_formula_sum        'C64 H93 Mn6 N24 O32.50 S8'
_cod_database_code               7247331
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Restrained distances
 S5-C30
 1.78 with sigma of 0.01
 S4-C31 = S4-C32
 1.78 with sigma of 0.01
 S3-O16 = S4-O17
 1.5 with sigma of 0.01
 S3-C33 = S3-C34 = S4-C31 = S4-C32
 1.78 with sigma of 0.01
 S5-O18 = S6-O19
 1.5 with sigma of 0.01
 S6-C36 = S5-C29 = S5-C30 = S6-C35
 1.78 with sigma of 0.01
 O16-H14A
 1.8 with sigma of 0.01
 C29-C30
 2.7 with sigma of 0.01
 O17-C31 = O17-C32
 2.65 with sigma of 0.01
 S4-C31 \\sim S4-C32
 with sigma of 0.02
 S3-O16 \\sim S4-O17
 with sigma of 0.02
 S3-C33 \\sim S3-C34 \\sim S4-C31 \\sim S4-C32
 with sigma of 0.02
 S5-O18 \\sim S6-O19
 with sigma of 0.02
 S5-C29 \\sim S6-C36 \\sim S5-C30 \\sim S6-C35
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O16, S3, C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 S4, O17, C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 S6, C35, C36, O19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O18, S5, C29, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: S5(0.6) S4(0.7) O17(0.7) O18(0.6) C29(0.6) H29A(0.6) H29B(0.6)
 H29C(0.6) C30(0.6) H30A(0.6) H30B(0.6) H30C(0.6) C31(0.7) H31A(0.7) H31B(0.7)
 H31C(0.7) C32(0.7) H32A(0.7) H32B(0.7) H32C(0.7) O14(0.42) H14A(0.42)
 H14B(0.42) S3(0.3) C33(0.3) H33A(0.3) H33B(0.3) H33C(0.3) C34(0.3) H34A(0.3)
 H34B(0.3) H34C(0.3) O16(0.3) S6(0.4) C35(0.4) H35A(0.4) H35B(0.4) H35C(0.4)
 C36(0.4) H36A(0.4) H36B(0.4) H36C(0.4) O19(0.4) O20(0.25) H20A(0.25)
 H20B(0.25) O15(0.58) H15A(0.58) H15B(0.58)
5.a Free rotating group:
 O14(H14A,H14B), O20(H20A,H20B), O15(H15A,H15B)
5.b Rotating group:
 O10(H10A,H10B), O3(H3A,H3B), O2(H2A,H2B), O11(H11A,H11B), O7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C12(H12), C14(H14), C18(H18), C22(H22), C23(H23),
 C24(H24), C26(H26)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              37708
_olex2_submission_special_instructions 'No special instructions were received'