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_7706488
_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 N4 Zn'
_chemical_formula_sum            'C29 H22 Br F5 N4 Zn'
_chemical_formula_weight         666.78
_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                86.721(2)
_cell_angle_beta                 86.179(2)
_cell_angle_gamma                84.625(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8072(2)
_cell_length_b                   11.5434(3)
_cell_length_c                   12.0315(2)
_cell_measurement_reflns_used    15378
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.9100
_cell_measurement_theta_min      3.5500
_cell_volume                     1351.28(5)
_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    -39.00  51.00   1.00    6.00    --  -17.55  57.00  90.00   90
  2  \w    -48.00  39.00   1.00    6.00    --  -17.55  77.00-120.00   87
  3  \w     -2.00  88.00   1.00    6.00    --   19.26  57.00-150.00   90
  4  \w     -2.00  88.00   1.00    6.00    --   19.26  57.00 -60.00   90
  5  \w     -2.00  88.00   1.00    6.00    --   19.26  57.00  30.00   90
  6  \w     -2.00  88.00   1.00    6.00    --   19.26  57.00 120.00   90
  7  \w    -20.00  61.00   1.00    6.00    --   19.26 -99.00  30.00   81
  8  \w    -39.00  49.00   1.00    6.00    --   19.26 -77.00 150.00   88
  9  \w    -50.00  41.00   1.00    6.00    --   19.26 -57.00 -30.00   91
 10  \w    -93.00 -39.00   1.00    6.00    --  -17.55-178.00 -90.00   54
 11  \w    -20.00  61.00   1.00    6.00    --   19.26 -99.00 150.00   81
 12  \w    -20.00  61.00   1.00    6.00    --   19.26 -99.00 -90.00   81
 13  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00-180.00  146
 14  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00-150.00  146
 15  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00-120.00  146
 16  \w    -11.00  39.00   1.00    6.00    --   19.26  77.00  60.00   50
 17  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00 -60.00  146
 18  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00 -30.00  146
 19  \w    -54.00  82.00   1.00    6.00    --   19.26   0.00   0.00  136
 20  \w    -54.00  92.00   1.00    6.00    --   19.26   0.00 -90.00  146
;
_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      0.0719006000
_diffrn_orient_matrix_UB_12      -0.0146080000
_diffrn_orient_matrix_UB_13      -0.0058816000
_diffrn_orient_matrix_UB_21      -0.0102079000
_diffrn_orient_matrix_UB_22      -0.0595726000
_diffrn_orient_matrix_UB_23      0.0118884000
_diffrn_orient_matrix_UB_31      -0.0048353000
_diffrn_orient_matrix_UB_32      -0.0075405000
_diffrn_orient_matrix_UB_33      -0.0576566000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0269
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            51141
_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         25.350
_diffrn_reflns_theta_min         3.238
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.449
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.992
_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 brownish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_preparation       'Transmetallation ofn lithium salt'
_exptl_crystal_recrystallization_method
'slow evaporation from a diluted n-hexane solution'
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0349P)^2^+1.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4347
_reflns_number_total             4931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00175b2.cif
_cod_data_source_block           j2008_347
_cod_depositor_comments
'Adding full bibliography for 7706485--7706489.cif.'
_cod_database_code               7706488
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H22 F5 N4 Zn1 Br1'
_chemical_oxdiff_usercomment     '@ 190 K'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C1(H1), C24(H24), C22(H22), C11(H11), C21(H21), C10(H10), C3(H3),
 C29(H29), C2(H2)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              19169
_shelx_hkl_checksum              51127
_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 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.877