Metal coordination induced ring contraction of porphyrin derivatives.
Patra, Bratati; Sobottka, Sebastian; Mondal, Sruti; Sarkar, Biprajit; Kar, Sanjib; Chemical communications (Cambridge, England) 54 (2018) 9945–9948; doi:10.1039/c8cc04670k

data_7122133
_publ_section_title
;
 Metal coordination induced ring contraction of porphyrin derivatives.
;
_journal_issue                   71
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9945
_journal_page_last               9948
_journal_paper_doi               10.1039/c8cc04670k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '3(C43 H25 Ag Fe N6)'
_chemical_formula_sum            'C129 H75 Ag3 Fe3 N18'
_chemical_formula_weight         2368.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-23
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2018-05-10 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.222(2)
_cell_angle_beta                 104.379(2)
_cell_angle_gamma                117.221(4)
_cell_formula_units_Z            2
_cell_length_a                   18.4767(6)
_cell_length_b                   18.7775(7)
_cell_length_c                   19.6170(5)
_cell_measurement_reflns_used    34265
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      77.1110
_cell_measurement_theta_min      2.7650
_cell_volume                     5558.5(4)
_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      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -42.00  30.00   0.50    4.00    --  -38.50  29.00  98.00  144
  2  \w   -101.00 -58.00   0.50    4.00    --  -38.50 -29.00 -61.00   86
  3  \w    -17.00  35.00   0.50    4.00    --   49.06 -29.00 -61.00  104
  4  \w     64.00 109.00   0.50    4.00    --   49.06  29.00  98.00   90
  5  \w     38.00 108.00   0.50   16.00    --  106.38 -29.00 -61.00  140
  6  \w    104.00 173.00   0.50   16.00    --  106.38  29.00  98.00  138
  7  \w   -100.00 -32.00   0.50    4.00    --  -38.50 -57.00 -90.00  136
  8  \w   -105.00 -38.00   0.50    4.00    --  -38.50 -19.00 -30.00  134
  9  \w    -77.00  -6.00   0.50    4.00    --  -38.50 125.00  30.00  142
 10  \w     56.00 100.00   0.50    4.00    --   49.06-125.00   0.00   88
 11  \w     26.00  97.00   0.50    4.00    --   49.06-125.00-150.00  142
 12  \w      2.00  49.00   0.50    4.00    --   49.06 -37.00-150.00   94
 13  \w     48.00 130.00   0.50   16.00    --  106.38 -77.00-180.00  164
 14  \w     45.00 113.00   0.50   16.00    --  106.38 -61.00  30.00  136
 15  \w    136.00 170.00   0.50   16.00    --  106.38 125.00   0.00   68
 16  \w     44.00  91.00   0.50   16.00    --  106.38 -61.00 -90.00   94
 17  \w    112.00 154.00   0.50   16.00    --  106.38  45.00 120.00   84
 18  \w     46.00  73.00   0.50   16.00    --  106.38 -30.00-150.00   54
 19  \w     66.00 122.00   0.50   16.00    --  106.38-125.00 -60.00  112
 20  \w     81.00 109.00   0.50   16.00    --  106.38 -94.00  60.00   56
 21  \w     45.00  72.00   0.50   16.00    --  106.38 -94.00-180.00   54
 22  \w     49.00 102.00   0.50   16.00    --  106.38 -94.00 -30.00  106
 23  \w     43.00 111.00   0.50   16.00    --  106.38 -45.00 -60.00  136
 24  \w     43.00 111.00   0.50   16.00    --  106.38 -45.00-180.00  136
 25  \w    118.00 145.00   0.50   16.00    --  106.38  30.00  60.00   54
 26  \w     45.00 111.00   0.50   16.00    --  106.38 -45.00  30.00  132
 27  \w     38.00 115.00   0.50   16.00    --  106.38 -15.00  90.00  154
 28  \w     50.00  94.00   0.50   16.00    --  106.38 -77.00 -30.00   88
 29  \w     41.00 105.00   0.50   16.00    --  106.38 -30.00  90.00  128
 30  \w    103.00 171.00   0.50   16.00    --  106.38  45.00  60.00  136
 31  \w    105.00 135.00   0.50   16.00    --  106.38  45.00 -30.00   60
 32  \w     84.00 109.00   0.50   16.00    --  106.38 -30.00-150.00   50
 33  \w     42.00 119.00   0.50   16.00    --  106.38-125.00-120.00  154
 34  \w     96.00 134.00   0.50   16.00    --  106.38 125.00   0.00   76
 35  \w     76.00 103.00   0.50   16.00    --  106.38 -45.00 150.00   54
 36  \w     87.00 119.00   0.50   16.00    --  106.38-125.00  60.00   64
 37  \w     77.00 104.00   0.50   16.00    --  106.38 -94.00 120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0741563000
_diffrn_orient_matrix_UB_12      0.0345284000
_diffrn_orient_matrix_UB_13      -0.0304721000
_diffrn_orient_matrix_UB_21      -0.0168437000
_diffrn_orient_matrix_UB_22      0.0712668000
_diffrn_orient_matrix_UB_23      -0.0109202000
_diffrn_orient_matrix_UB_31      0.0661233000
_diffrn_orient_matrix_UB_32      0.0565514000
_diffrn_orient_matrix_UB_33      0.0791444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.999
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         2.452
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32705
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1378
_refine_ls_number_reflns         19796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0533
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16557
_reflns_number_total             19796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04670k2.cif
_cod_data_source_block           skar_fer_ag1
_cod_depositor_comments
'Adding full bibliography for 7122132--7122133.cif.'
_cod_database_code               7122133
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C246 H172 Ag6 Fe6 N62 '
_diffrn_oxdiff_ac3_digest_frames
;
01cadc4385ce8e85668056279266ee080d00026fea7
;
_diffrn_oxdiff_ac3_digest_hkl
;
0137b3052fe83395b2a64bef27b17d7484f2af
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C12(H12), C13(H13), C17(H17), C12B(H12B), C42(H42), C2A(H2A),
 C17B(H17B), C3(H3), C2(H2), C3B(H3B), C28B(H28B), C18A(H18A), C17A(H17A),
 C8(H8), C8B(H8B), C18(H18), C38(H38), C7A(H7A), C8A(H8A), C38B(H38B),
 C28A(H28A), C7B(H7B), C25(H25), C13A(H13A), C41(H41), C42A(H42A), C13B(H13B),
 C39(H39), C7(H7), C31A(H31A), C42B(H42B), C21A(H21A), C39A(H39A), C41A(H41A),
 C41B(H41B), C24A(H24A), C25A(H25A), C2B(H2B), C28(H28), C31B(H31B), C24(H24),
 C18B(H18B), C25B(H25B), C38A(H38A), C12A(H12A), C30A(H30A), C22A(H22A),
 C29B(H29B), C39B(H39B), C31(H31), C35B(H35B), C34B(H34B), C33B(H33B),
 C29A(H29A), C36B(H36B), C24B(H24B), C21B(H21B), C29(H29), C32B(H32B), C21(H21),
  C34(H34), C22B(H22B), C30(H30), C30B(H30B), C36(H36), C22(H22), C33(H33),
 C35A(H35A), C35(H35), C32(H32), C32A(H32A), C34A(H34A), C33A(H33A), C36A(H36A)
;
_shelx_res_checksum              58051
_shelx_fab_checksum              1189
_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 2.932
_oxdiff_exptl_absorpt_empirical_full_min 0.409