Coordination-Induced Spin-State Switching with Nickel Chlorin and Nickel Isobacteriochlorin.
Dommaschk, Marcel; Thoms, Vanessa; Schütt, Christian; Näther, Christian; Puttreddy, Rakesh; Rissanen, Kari; Herges, Rainer; Inorganic chemistry 54 (2015) 9390–9392; doi:10.1021/acs.inorgchem.5b01756

data_4344151
_publ_section_title
;
 Coordination-Induced Spin-State Switching with Nickel Chlorin and Nickel
 Isobacteriochlorin.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9390
_journal_page_last               9392
_journal_paper_doi               10.1021/acs.inorgchem.5b01756
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '3(C57 H26 F20 N7 Ni), 5(C5 H5 N)'
_chemical_formula_sum            'C196 H103 F60 N26 Ni3'
_chemical_formula_weight         4138.17
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1895(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.4208(3)
_cell_length_b                   16.22196(18)
_cell_length_c                   26.4999(4)
_cell_measurement_reflns_used    10166
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.7540
_cell_measurement_theta_min      4.2990
_cell_volume                     8755.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega -101.00  -20.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -37.0000 -150.0000 162

  2 omega -108.00  -12.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -19.0000  -90.0000 192

  3 omega  125.00  152.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  125.0000 -180.0000 54

  4 omega   35.00   90.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  -30.0000 -120.0000 110

  5 omega   39.00   98.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  -45.0000  -60.0000 118

  6 omega   85.00  174.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642   61.0000 -120.0000 178

  7 omega   94.00  120.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  125.0000 -180.0000 52

  8 omega   57.00   93.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  -94.0000  -60.0000 72

  9 omega   41.00  138.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8642  -61.0000   90.0000 194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0000040000
_diffrn_orient_matrix_UB_12      -0.0393510000
_diffrn_orient_matrix_UB_13      -0.0529638000
_diffrn_orient_matrix_UB_21      0.0738055000
_diffrn_orient_matrix_UB_22      0.0188322000
_diffrn_orient_matrix_UB_23      -0.0010443000
_diffrn_orient_matrix_UB_31      0.0165586000
_diffrn_orient_matrix_UB_32      -0.0842549000
_diffrn_orient_matrix_UB_33      0.0244690000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27157
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.747
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       needle
_exptl_crystal_F_000             4170
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.0421
_exptl_crystal_size_min          0.0291
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1320
_refine_ls_number_reflns         15394
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1317P)^2^+12.6599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12551
_reflns_number_total             15394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01756_si_002.cif
_cod_data_source_block           nitpcf20-2py_(2*2Py)
_cod_depositor_comments
'Adding full bibliography for 4344148--4344152.cif.'
_cod_database_code               4344151
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C60 H30 N7 F20 Ni1'
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C59, C59A}
{C60, C60A}
3. Uiso/Uaniso restraints and constraints
Uanis(C89) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C90) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C98) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C59) = Uanis(C59A)
Uanis(C60) = Uanis(C60A)
4. Others
 Fixed Sof: N11(0.5) H11(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5) C68(0.5)
 H68A(0.5) H68B(0.5) C69(0.5) H69A(0.5) H69B(0.5) C70(0.5) H70A(0.5) H70B(0.5)
 H70C(0.5) C98(0.5) H98(0.5) C99(0.5) H99(0.5) C100(0.5) H100(0.5) C101(0.5)
 H101(0.5) C102(0.5) H102(0.5) N14(0.5) C59A(0.5) H59A(0.5) C60A(0.5) H60A(0.5)
5.a Ternary CH refined with riding coordinates:
 N7(H7), C12(H12), C13(H13), N11(H11), C59(H59), C60(H60)
5.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C68(H68A,H68B), C69(H69A,H69B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7A), C8(H8), C17(H17), C18(H18), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C64(H64), C65(H65), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C88(H88), C89(H89),
 C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97),
  C59A(H59A), C60A(H60A)
5.d Fitted hexagon refined as free rotating group:
 C98(C99,C100,C101,C102,N14)
5.e Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              77603
_shelx_hkl_checksum              79238
_olex2_submission_special_instructions 'No special instructions were received'