Nickel(ii) monobenzoporphyrins and chlorins: synthesis, electrochemistry and anion sensing properties
Kumar, Sandeep; Chaudhri, Nivedita; Osterloh, W. Ryan; Kadish, Karl M.; Sankar, Muniappan; Dalton Transactions  (2021) –; doi:10.1039/D1DT03122H

data_7708821
_publ_section_title
;
 Nickel(ii) monobenzoporphyrins and chlorins: synthesis, electrochemistry
 and anion sensing properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03122H
_journal_year                    2021
_chemical_formula_moiety         'C70 H38 N4 Ni O8, C H Cl3'
_chemical_formula_sum            'C71 H39 Cl3 N4 Ni O8'
_chemical_formula_weight         1241.12
_chemical_name_common            NiDFP(IND)2(Benzo)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.788(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.865(2)
_cell_length_b                   18.0617(19)
_cell_length_c                   14.9964(15)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.340
_cell_measurement_theta_min      0.98
_cell_volume                     5622.7(10)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            80220
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.344
_diffrn_reflns_theta_min         0.981
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square shaped'
_exptl_crystal_F_000             2544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform/hexane'
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.989
_exptl_transmission_factor_min   0.989
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         13968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1147P)^2^+4.7002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8745
_reflns_number_total             13968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03122h2.cif
_cod_data_source_block           ups3759ms_skniindbr4_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5622.8(10)
_cod_database_code               7708821
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.989
_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 Ternary CH refined with riding coordinates:
 C71(H71)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C4(H4), C49(H49), C63(H63), C46(H46), C22(H22), C24(H24),
 C66(H66), C25(H25), C52(H52), C62(H62), C14(H14), C48(H48), C47(H47), C23(H23),
  C56(H56), C58(H58), C59(H59), C61(H61), C55(H55), C60(H60), C39(H39),
 C54(H54), C53(H53), C33(H33), C30(H30), C32(H32), C42(H42), C40(H40), C31(H31),
  C41(H41)
2.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              44326
_shelx_hkl_checksum              65175