Synthesis and complexes of a constrained-cavity Schiff-base dipyrrin macrocycle.
van Rees, Karlotta; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1610–1613; doi:10.1039/d1dt00175b

data_7706487
_publ_section_title
;
 Synthesis and complexes of a constrained-cavity Schiff-base dipyrrin
 macrocycle.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1610
_journal_page_last               1613
_journal_paper_doi               10.1039/d1dt00175b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C29 H22 Br F5 Fe N4, C H2 Cl2'
_chemical_formula_sum            'C30 H24 Br Cl2 F5 Fe N4'
_chemical_formula_weight         742.19
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                108.864(6)
_cell_angle_beta                 98.831(6)
_cell_angle_gamma                90.523(5)
_cell_formula_units_Z            2
_cell_length_a                   9.6171(6)
_cell_length_b                   12.2102(9)
_cell_length_c                   13.8745(10)
_cell_measurement_reflns_used    4462
_cell_measurement_temperature    170
_cell_measurement_theta_max      21.0380
_cell_measurement_theta_min      3.8540
_cell_volume                     1520.44(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_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      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  25.00   1.00   22.50    --  -17.39 -99.00 -30.00   45
  2  \w     -2.00  88.00   1.00   22.50    --   19.11  57.00 120.00   90
  3  \w     -7.00  92.00   1.00   22.50    --   19.11  37.00 -30.00   99
  4  \w    -39.00  49.00   1.00   22.50    --   19.11 -77.00 -30.00   88
  5  \w    -20.00  61.00   1.00   22.50    --   19.11 -99.00  90.00   81
  6  \w    -20.00  61.00   1.00   22.50    --   19.11 -99.00-180.00   81
  7  \w     -7.00  92.00   1.00   22.50    --   19.11  37.00-120.00   99
  8  \w     -7.00  92.00   1.00   22.50    --   19.11  37.00  30.00   99
  9  \w    -50.00  41.00   1.00   22.50    --   19.11 -57.00-150.00   91
 10  \w    -93.00 -39.00   1.00   22.50    --  -17.39-178.00  30.00   54
 11  \w    -39.00  13.00   1.00   22.50    --  -17.39 -77.00 -90.00   52
 12  \w     -2.00  88.00   1.00   22.50    --   19.11  57.00-180.00   90
 13  \w    -20.00  61.00   1.00   22.50    --   19.11 -99.00   0.00   81
 14  \w    -11.00  39.00   1.00   22.50    --   19.11  77.00-180.00   50
 15  \w    -54.00  92.00   1.00   22.50    --   19.11   0.00-180.00  146
 16  \w    -20.00  61.00   1.00   22.50    --   19.11 -99.00 -90.00   81
 17  \w    -54.00  92.00   1.00   22.50    --   19.11   0.00-120.00  146
 18  \w    -54.00  -4.00   1.00   22.50    --   19.11   0.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107277000
_diffrn_orient_matrix_UB_12      0.0588554000
_diffrn_orient_matrix_UB_13      0.0036594000
_diffrn_orient_matrix_UB_21      -0.0671783000
_diffrn_orient_matrix_UB_22      -0.0030488000
_diffrn_orient_matrix_UB_23      -0.0304789000
_diffrn_orient_matrix_UB_31      -0.0310645000
_diffrn_orient_matrix_UB_32      0.0176114000
_diffrn_orient_matrix_UB_33      0.0453687000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1238
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41369
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull bluish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_preparation       'Transmetallation with the lithium salt'
_exptl_crystal_recrystallization_method
'Slow evaporation of a diluted n-hexane solution'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0535P)^2^+4.4748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4175
_reflns_number_total             5570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00175b2.cif
_cod_data_source_block           j2008_239_1
_cod_depositor_comments
'Adding full bibliography for 7706485--7706489.cif.'
_cod_database_code               7706487
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H22 F5 N4 Fe1 Br1'
_chemical_oxdiff_usercomment     '@ 190 K'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.034) H24(0.034) H8(0.031) H10(0.033) H11(0.033) H21(0.038)
 H22(0.042) H6A(0.05) H6B(0.05) H6C(0.05) H7A(0.058) H7B(0.058) H7C(0.058)
 H30A(0.06) H30B(0.06) H2(0.051) H29(0.046) H3(0.044) H26A(0.066) H26B(0.066)
 H26C(0.066) H27A(0.075) H27B(0.075) H27C(0.075)
 Fixed X: H1(0.063431) H24(0.113115) H8(0.281714) H10(0.344969) H11(0.347949)
 H21(0.227883) H22(0.156814) H6A(-0.02415) H6B(0.019216) H6C(0.020095)
 H7A(0.260306) H7B(0.280625) H7C(0.386352) H30A(0.62738) H30B(0.475883)
 H2(0.427951) H29(0.308144) H3(0.388965) H26A(-0.103662) H26B(-0.077188) H26C(-
 0.092838) H27A(0.255254) H27B(0.149758) H27C(0.100537)
 Fixed Y: H1(0.773534) H24(0.790207) H8(0.5055) H10(0.273465) H11(0.194875)
 H21(0.393322) H22(0.591483) H6A(0.696554) H6B(0.76976) H6C(0.631315)
 H7A(0.634044) H7B(0.772578) H7C(0.698774) H30A(0.614206) H30B(0.557943)
 H2(1.048679) H29(1.050971) H3(0.897472) H26A(0.883766) H26B(0.973376)
 H26C(0.837008) H27A(0.964306) H27B(1.056268) H27C(0.967875)
 Fixed Z: H1(0.432039) H24(0.119807) H8(0.557763) H10(0.427064) H11(0.237727)
 H21(-0.067648) H22(-0.057818) H6A(0.532758) H6B(0.652717) H6C(0.614962)
 H7A(0.69306) H7B(0.736244) H7C(0.665478) H30A(0.29158) H30B(0.228199)
 H2(0.605916) H29(0.449197) H3(0.667692) H26A(0.236072) H26B(0.35143)
 H26C(0.33207) H27A(0.258232) H27B(0.312191) H27C(0.197773)
;
_shelx_res_checksum              18535
_shelx_hkl_checksum              15462
_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 1.089
_oxdiff_exptl_absorpt_empirical_full_min 0.923