Deciphering supramolecular isomerization in coordination polymers: connected molecular squares <i>vs.</i> fused hexagons.
Gupta, Vijay; Laha, Biswajit; Khullar, Sadhika; Mandal, Sanjay K.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2221–2232; doi:10.1039/d0dt04196c

data_7706172
_publ_section_title
;
 Deciphering supramolecular isomerization in coordination polymers:
 connected molecular squares <i>vs.</i> fused hexagons.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2221
_journal_page_last               2232
_journal_paper_doi               10.1039/d0dt04196c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C60 H56 Mn2 N6 O14, 6(H2 O) (C2 H6 O)'
_chemical_formula_sum            'C62 H74 Mn2 N6 O21'
_chemical_formula_weight         1349.15
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-26 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                69.652(7)
_cell_angle_beta                 87.876(7)
_cell_angle_gamma                71.709(7)
_cell_formula_units_Z            1
_cell_length_a                   9.879(4)
_cell_length_b                   12.369(4)
_cell_length_c                   14.629(5)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.36
_cell_volume                     1586.1(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 2013.4_1 (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21781
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.151
_diffrn_reflns_theta_max         25.151
_diffrn_reflns_theta_min         2.178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0627 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.9191. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5646
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0301P)^2^+0.9553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5014
_reflns_number_total             5646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04196c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7706167--7706173.cif.'
_cod_original_cell_volume        1586.2(10)
_cod_database_code               7706172
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H20A,H20B} of C20, {H27A,H27B} of C27, {H21A,H21B} of C21
 At 1.5 times of:
  All O(H,H) groups, {H6A,H6B} of C3
2. Restrained distances
 O6_$1-H6B_$1
 0.82 with sigma of 0.01
 O6_$1-H6A_$1
 0.82 with sigma of 0.01
 O10-H10A = O10-H10B
 0.87 with sigma of 0.02
 O9-H9A = O9-H9B
 0.87 with sigma of 0.02
 O8-H8A = O8-H8B
 0.87 with sigma of 0.02
 H10A-H10B
 1.38 with sigma of 0.04
 H9A-H9B
 1.38 with sigma of 0.04
 H8A-H8B
 1.38 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29),
  C30(H30)
;
_shelx_res_checksum              56459
_shelx_fab_checksum              28419
_olex2_submission_special_instructions 'No special instructions were received'