Synthesis and characterization of a dual-stimuli-responsive cobalt(iii) complex: comparison of photo-/thermo-mechanical behaviour in crystal and polymer composites
Singh, Manjeet; Narang, Karan Kumar; Kaur, Yashpreet; Patra, Ranjan; Nanda, Prasant K.; Sahoo, Subash C.; CrystEngComm 26 (2024) 5004–5012; doi:10.1039/D4CE00638K

data_7249182
_publ_section_title
;
 Synthesis and characterization of a dual-stimuli-responsive cobalt(iii)
 complex: comparison of photo-/thermo-mechanical behaviour in crystal and
 polymer composites
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5004
_journal_page_last               5012
_journal_paper_doi               10.1039/D4CE00638K
_journal_volume                  26
_journal_year                    2024
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C9 H6 N O4), Co H15 N6 O2, 2(H2 O)'
_chemical_formula_sum            'C18 H31 Co N8 O12'
_chemical_formula_weight         610.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0239(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2165(3)
_cell_length_b                   6.20030(11)
_cell_length_c                   28.4449(5)
_cell_measurement_reflns_used    20506
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2720
_cell_measurement_theta_min      3.3570
_cell_volume                     2505.76(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -80.00 -55.00   0.50    5.00    --   -9.95 169.00 -44.00   50
  2  \w    -52.00   5.00   0.50    5.00    --   -9.95 115.00 171.00  114
  3  \w     12.00  52.00   0.50    5.00    --   10.22-115.00  82.00   80
  4  \w     31.00  57.00   0.50    5.00    --   10.22-169.00 -61.00   52
  5  \w    -19.00  52.00   0.50    5.00    --   -9.95  38.00 -30.00  142
  6  \w     19.00  53.00   0.50    5.00    --   -9.95  57.00   0.00   68
  7  \w    -22.00  60.00   0.50    5.00    --   -9.95  19.00  90.00  164
  8  \w    -17.00   9.00   0.50    5.00    --   -9.95  57.00   0.00   52
  9  \w     -9.00  50.00   0.50    5.00    --   -9.95  38.00   0.00  118
 10  \w    -58.00 -33.00   0.50    5.00    --   -9.95 125.00  90.00   50
 11  \w    -20.00   5.00   0.50    5.00    --   -9.95  38.00 120.00   50
 12  \w     17.00  51.00   0.50    5.00    --   -9.95  38.00 120.00   68
 13  \w    -56.00 -22.00   0.50    5.00    --   -9.95 125.00 -60.00   68
 14  \w    -44.00 -19.00   0.50    5.00    --   -9.95 125.00-120.00   50
 15  \w      5.00  54.00   0.50    5.00    --   10.22-125.00 -60.00   98
 16  \w    -37.00  -6.00   0.50    5.00    --   10.22 128.00 135.90   62
 17  \w    -31.00   1.00   0.50    5.00    --   10.22 118.00 -25.06   64
 18  \w     -8.00  74.00   0.50    5.00    --   10.22  57.00-180.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0386677000
_diffrn_orient_matrix_UB_12      0.0097751000
_diffrn_orient_matrix_UB_13      0.0149403000
_diffrn_orient_matrix_UB_21      -0.0315311000
_diffrn_orient_matrix_UB_22      -0.0168621000
_diffrn_orient_matrix_UB_23      -0.0195386000
_diffrn_orient_matrix_UB_31      0.0013872000
_diffrn_orient_matrix_UB_32      -0.1127260000
_diffrn_orient_matrix_UB_33      0.0042282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33972
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.348
_diffrn_reflns_theta_min         3.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0548
_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^)+14.1336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4948
_reflns_number_total             5424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00638k11.cif
_cod_data_source_block           C-1
_cod_depositor_comments          'Adding full bibliography for 7249182.cif.'
_cod_original_cell_volume        2505.75(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249182
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Co C H N O'
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 C16, C17
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17A, C16A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
2. Others
 Fixed Sof: C17(0.8) H17(0.8) C16(0.8) H16(0.8) C16A(0.2) H16A(0.2) C17A(0.2)
 H17A(0.2)
3.a Free rotating group:
 O11(H11A,H11B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C5(H5), C2(H2), C8(H8), C11(H11), C15(H15), C12(H12),
 C17(H17), C16(H16), C14(H14), C16A(H16A), C17A(H17A)
3.c Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N6(H6A,H6B,H6C), N5(H5A,H5B,H5C), N2(H2A,H2B,H2C), N3(H3A,
 H3B,H3C)
;
_shelx_res_checksum              16592
_shelx_hkl_checksum              91954
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.735