Protecting the triplet excited state in sterically congested platinum porphyrin.
Moiseev, A. G.; Margulies, E. A.; Schneider, J. A.; Bélanger-Gariépy, F; Perepichka, D. F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2676–2683; doi:10.1039/c3dt52926f

data_7029526
_publ_section_title
;
 Protecting the triplet excited state in sterically congested platinum
 porphyrin.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2676
_journal_page_last               2683
_journal_paper_doi               10.1039/c3dt52926f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C68 H76 N4 Pt, 2(C2 H6 O)'
_chemical_formula_sum            'C72 H88 N4 O2 Pt'
_chemical_formula_weight         1236.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4707)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8481(5)
_cell_length_b                   28.8481(5)
_cell_length_c                   14.8117(3)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.762
_cell_measurement_theta_min      3.063
_cell_volume                     12326.5(4)
_computing_cell_refinement
;
SAINT (2009) V7.68A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2009) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2009) V7.68A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Quazar MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            119240
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.054
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'Microfocus Source'
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mS High Brilliance Microsource'
_exptl_absorpt_coefficient_mu    4.623
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.5957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0441 after correction.
The Ratio of minimum to maximum transmission is 0.7907.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5936
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0501P)^2^+29.3687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5397
_reflns_number_total             5936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52926f.txt
_cod_data_source_block           pere28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_crystal_colour_primary' value 'Pink' changed to
'pink' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        12326.5(5)
_cod_database_code               7029526
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C21-C22 \\sim C21-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(O61A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C63A) \\sim Ueq,
Uanis(O61B) \\sim Ueq, Uanis(C62B) \\sim Ueq, Uanis(C63B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C63A) = Uanis(C63B)
Uanis(C62A) = Uanis(C62B)
Uanis(O61A) = Uanis(O61B)
Uanis(C22) = Uanis(C42)
Uanis(C23) = Uanis(C43)
Uanis(C24) = Uanis(C44)
Uanis(C25) = Uanis(C45)
Uanis(C26) = Uanis(C46)
Uanis(C27) = Uanis(C47)
Uanis(C28) = Uanis(C48)
Uanis(C29) = Uanis(C49)
Uanis(C30) = Uanis(C50)
Uanis(C31) = Uanis(C51)
Uanis(C32) = Uanis(C52)
Uanis(C33) = Uanis(C53)
Uanis(C34) = Uanis(C54)
4. Same fragment restrains
{C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34}
as
{C43, C44, C45, C46, C47, C48, C49, C50, C51, C52, C53, C54}
{O61A, C62A, C63A}
as
{O61B, C62B, C63B}
5. Others
 Sof(C43)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(C47)=Sof(H47)=Sof(C48)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(1)
 Sof(C23)=Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(H21C)=Sof(H21D)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(2)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Sof(O61B)=Sof(H61B)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C63B)=Sof(H63D)=
 Sof(H63E)=Sof(H63F)=1-FVAR(3)
 Sof(O61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(C63A)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C21(H21C,H21D), C29(H29A,
 H29B), C31(H31A,H31B), C33(H33A,H33B), C49(H49A,H49B), C51(H51A,H51B),
 C53(H53A,H53B), C62A(H62A,H62B), C62B(H62C,H62D)
6.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C42(H42A,H42B,
 H42C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C50(H50A,H50B,H50C), C54(H54A,
 H54B,H54C), C63A(H63A,H63B,H63C), C63B(H63D,H63E,H63F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C13(H13), C15(H15), C25(H25), C27(H27),
 C45(H45), C47(H47)
6.d Tetrahedral OH refined with riding coordinates:
 O61A(H61A), O61B(H61B)
6.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C52(H52A,H52B,H52C)
;