Determining the key vibrations for spin relaxation in ruffled Cu(ii) porphyrins <i>via</i> resonance Raman spectroscopy.
Kazmierczak, Nathanael P.; Lopez, Nathan E.; Luedecke, Kaitlin M.; Hadt, Ryan G.; Chemical science 15 (2024) 2380–2390; doi:10.1039/d3sc05774g

data_1570769
_publ_section_title
;
 Determining the key vibrations for spin relaxation in ruffled Cu(ii)
 porphyrins <i>via</i> resonance Raman spectroscopy.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2380
_journal_page_last               2390
_journal_paper_doi               10.1039/d3sc05774g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C130 H148 Cl4 Cu4 N16'
_chemical_formula_weight         2330.60
_chemical_name_systematic
'copper tetraisopropylporphyrin dichloromethane solvate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2024-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8836(4)
_cell_length_b                   10.8836(4)
_cell_length_c                   47.541(5)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.51
_cell_measurement_theta_min      3.72
_cell_volume                     5631.4(7)
_computing_cell_refinement       'SAINT v8.40A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker Nano, 2020)'
_computing_data_reduction        'SAINT v8.40A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.69
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            42982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.585
_diffrn_reflns_theta_min         1.858
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2448
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / hexanes'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
; 
 Twinning involves inversion, so Flack parameter cannot be determined 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         5789
_refine_ls_number_restraints     2028
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0711P)^2^+4.1943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5310
_reflns_number_total             5789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05774g2.cif
_cod_data_source_block           V23325
_cod_depositor_comments          'Adding full bibliography for 1570769.cif.'
_cod_database_code               1570769
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.811
_shelx_res_checksum              26238