The crystal structure of dimethyl 4,4′-(10,20-diphenylporphyrin-5,15-diyl)dibenzoate dichloromethane solvate, C49H36N4O4Cl2
Xiao, Ze-en; Wang, Yiqun; Cui, Hao; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 849–851; doi:10.1515/ncrs-2023-0233

data_8107580
_publ_section_title
;
 The crystal structure of dimethyl
 4,4&#x2032;-(10,20-diphenylporphyrin-5,15-diyl)dibenzoate dichloromethane
 solvate, C49H36N4O4Cl2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              849
_journal_page_last               851
_journal_paper_doi               10.1515/ncrs-2023-0233
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C H2 Cl2, C48 H34 N4 O4'
_chemical_formula_sum            'C49 H34 Cl2 N4 O4'
_chemical_formula_weight         813.70
_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     direct
_cell_angle_alpha                95.986(3)
_cell_angle_beta                 102.790(3)
_cell_angle_gamma                95.563(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3858(2)
_cell_length_b                   12.6484(4)
_cell_length_c                   12.7115(5)
_cell_measurement_reflns_used    4583
_cell_measurement_temperature    150
_cell_measurement_theta_max      75.8410
_cell_measurement_theta_min      4.6910
_cell_volume                     988.12(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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    -82.00 -29.00   1.00    1.00    --  -41.14 125.00 -90.00   53
  2  \w    -84.00  23.00   1.00    1.00    --  -41.14   0.00-120.00  107
  3  \w   -115.00 -29.00   1.00    1.00    --  -41.14 -38.00-150.00   86
  4  \w     33.00  84.00   1.00    1.00    --   41.14-125.00-150.00   51
  5  \w      1.00  61.00   1.00    1.00    --   41.14 -99.00  90.00   60
  6  \w     45.00 128.00   1.00    4.00    --  112.00 -61.00  60.00   83
  7  \w     74.00 101.00   1.00    4.00    --  112.00-125.00-180.00   27
  8  \w     71.00  98.00   1.00    4.00    --  112.00 -77.00-180.00   27
  9  \w     41.00 138.00   1.00    4.00    --  112.00 -61.00 -60.00   97
 10  \w    102.00 133.00   1.00    4.00    --  112.00 -45.00 150.00   31
 11  \w     86.00 177.00   1.00    4.00    --  112.00  30.00  30.00   91
 12  \w     39.00  85.00   1.00    4.00    --  112.00 -45.00 150.00   46
 13  \w     86.00 175.00   1.00    4.00    --  112.00  30.00 -30.00   89
 14  \w     79.00 117.00   1.00    4.00    --  112.00-125.00-150.00   38
 15  \w     43.00 117.00   1.00    4.00    --  112.00-125.00   0.00   74
 16  \w     46.00 143.00   1.00    4.00    --  112.00 -15.00   0.00   97
 17  \w     30.00  86.00   1.00    4.00    --  112.00 -94.00 -90.00   56
 18  \w     77.00 104.00   1.00    4.00    --  112.00 -94.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1809350000
_diffrn_orient_matrix_UB_12      0.0636219000
_diffrn_orient_matrix_UB_13      -0.0384551000
_diffrn_orient_matrix_UB_21      0.1406169000
_diffrn_orient_matrix_UB_22      0.0179880000
_diffrn_orient_matrix_UB_23      0.1171502000
_diffrn_orient_matrix_UB_31      0.0981941000
_diffrn_orient_matrix_UB_32      -0.1042118000
_diffrn_orient_matrix_UB_33      -0.0224865000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.034
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3969
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0839P)^2^+0.9324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3534
_reflns_number_total             3969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0233_suppl_001.cif
_cod_data_source_block           6
_cod_database_code               8107580
_chemical_oxdiff_formula         CHON
_chemical_oxdiff_usercomment     BJQ
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.555
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 Cl2S-C1S = Cl1S-C1S
 1.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(Cl1S) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
;
_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 1.994
_oxdiff_exptl_absorpt_empirical_full_min 0.564