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_7706168
_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         'C31 H34 Mn N3 O5 Si, C3 H7 N O'
_chemical_formula_sum            'C34 H41 Mn N4 O6 Si'
_chemical_formula_weight         684.74
_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             2020-07-13
_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                106.695(7)
_cell_angle_beta                 98.167(8)
_cell_angle_gamma                95.093(7)
_cell_formula_units_Z            2
_cell_length_a                   9.116(3)
_cell_length_b                   13.297(4)
_cell_length_c                   15.131(4)
_cell_measurement_reflns_used    3043
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      2.47
_cell_volume                     1722.7(9)
_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                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23041
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0798 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8735. 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    1.320
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6012
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.8070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3736
_reflns_number_total             6012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04196c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7706167--7706173.cif.'
_cod_original_cell_volume        1722.8(8)
_cod_database_code               7706168
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 C29A, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29A, C29, C30, C31, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(C30A)=Sof(H30C)=Sof(H30D)=FVAR(1)
 Fixed Sof: C29A(0.5) H29A(0.5) H29B(0.5) C29(0.5) H29C(0.5) H29D(0.5)
4.a Rotating group:
 O5(H5A,H5B)
4.b Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C22(H22A,H22B), C23(H23A,H23B), C29(H29C,H29D), C30(H30A,
 H30B), C31(H31A,H31B), C31(H31C,H31D), C30A(H30C,H30D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28),
  C34(H34)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              50380
_olex2_submission_special_instructions 'No special instructions were received'