Inducing ring distortions in unsubstituted metallophthalocyanines using axial N-heterocyclic carbenes.
Kidd, Steven R.; Zhou, Wen; Warren, Jeffrey J.; Leznoff, Daniel B.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6537–6546; doi:10.1039/d4dt00528g

data_7715462
_publ_section_title
;
 Inducing ring distortions in unsubstituted metallophthalocyanines using
 axial N-heterocyclic carbenes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6537
_journal_page_last               6546
_journal_paper_doi               10.1039/d4dt00528g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C41 H26 N10 Zn, 2(C7 H8)'
_chemical_formula_sum            'C55 H42 N10 Zn'
_chemical_formula_weight         908.35
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-12 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.751(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0211(4)
_cell_length_b                   15.8643(6)
_cell_length_c                   23.5955(9)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    189.99
_cell_measurement_theta_max      64.367
_cell_measurement_theta_min      3.357
_cell_volume                     4497.7(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      189.99
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker PHOTO-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74613
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        64.537
_diffrn_reflns_theta_max         64.537
_diffrn_reflns_theta_min         3.357
_diffrn_source_current           0.65
_diffrn_source_power             0.029133000000000003
_diffrn_source_voltage           44.82
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.6497
_exptl_absorpt_correction_T_min  0.4946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1547 before and 0.0985 after correction.
The Ratio of minimum to maximum transmission is 0.7613.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       Block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.055
_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     599
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0447P)^2^+3.6262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6234
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00528g2.cif
_cod_data_source_block           cu_sk_pc1_znpc_bnhc_gb_tol_0m_a
_cod_depositor_comments
'Adding full bibliography for 7715459--7715462.cif.'
_cod_database_code               7715462
_shelx_shelxl_version_number     2019/1
_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:
 C14(H14), C15(H15), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C1(H1), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C48(H48A,H48B,H48C), C55(H55A,H55B,
 H55C)
;
_shelx_res_checksum              78673
_olex2_submission_special_instructions 'No special instructions were received'