Investigation of easy-plane magnetic anisotropy in P-ligand square-pyramidal CoII single ion magnets
Konar, Sanjit; Mondal, Amit Kumar; Jover, Jesús; Ruiz, Eliseo; Chem. Commun.  (2017) –; doi:10.1039/C7CC02584J

data_7119978
_publ_section_title
;
 Investigation of easy-plane magnetic anisotropy in P-ligand
 square-pyramidal CoII single ion magnets
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02584J
_journal_year                    2017
_chemical_formula_moiety         'C59 H37 F4 Ir N7, Cl'
_chemical_formula_sum            'C59 H37 Cl F4 Ir N7'
_chemical_formula_weight         1147.60
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1mg8kx
_audit_creation_date             2015-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2016-11-10 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.188(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8286(9)
_cell_length_b                   18.6390(6)
_cell_length_c                   17.8263(6)
_cell_measurement_reflns_used    7897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.1440
_cell_measurement_theta_min      3.1580
_cell_volume                     6919.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32146
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.563
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         8047
_exptl_absorpt_coefficient_mu    4.461
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.541
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         13180
_refine_ls_number_restraints     1381
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1180P)^2^+4.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8047
_reflns_number_total             13180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02584j2.cif
_cod_data_source_block           jcz_150429_sq
_cod_database_code               7119978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C14A-C13 = C14-C13 = C16-C15A = C16-C15 = C17-C16 = C17-C12 = C13-C12
 1.388 with sigma of 0.02
 N7-C48 \\sim N7A-C48
 with sigma of 0.02
 N7A-C45A \\sim N7-C45
 with sigma of 0.02
 N7-C54 \\sim N7A-C54
 with sigma of 0.02
 F2A-C5A \\sim F2-C5
 with sigma of 0.02
 F4A-C14A \\sim F4-C14
 with sigma of 0.02
3. Restrained planarity
 C15A, C14A, C13, C12, C17, C15
 with sigma of 0.2
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(F2A) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F1) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(F4A) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51) = Uanis(C52) = Uanis(C53)
Uanis(C42A) = Uanis(C43A) = Uanis(C44A) = Uanis(C45A) = Uanis(C46A) =
Uanis(C47A)
Uanis(N7) = Uanis(N7A)
Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47)
Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59)
6. Others
 Sof(C43A)=Sof(C42A)=Sof(H42A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(N7A)=1-FVAR(1)
 Sof(N7)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C42)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44)=Sof(C45)=FVAR(1)
 Sof(H11A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=
 Sof(H9A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=Sof(F2A)=1-FVAR(2)
 Sof(F2)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(H8)=Sof(C7)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=FVAR(2)
 Sof(H13A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(F4A)=1-FVAR(3)
 Sof(F4)=Sof(H13)=Sof(C14)=Sof(C15)=Sof(H15)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C11(H11A), C10(H10), C9(H9), C8(H8), C2(H2), C4A(H4A), C4(H4),
 C13(H13A), C13(H13), C15A(H15A), C15(H15), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47), C43(H43),
 C44(H44), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C59(H59), C58(H58),
  C57(H57), C56(H56), C55(H55), C42A(H42A), C44A(H44A), C46A(H46A), C47A(H47A),
 C10A(H10A), C9A(H9A), C8A(H8A)
7.b Fitted hexagon refined as free rotating group:
 N1(C11,C10,C9,C8,C7), C2(C3,C4A,C5A,C6A,C1), C13(C14A,C15A,C16,C17,C12),
 C46(C47,C42,C43,C44,C45), C54(C59,C58,C57,C56,C55), C43A(C42A,C44A,C45A,C46A,
 C47A)
;
_shelx_res_checksum              33163
_shelx_fab_checksum              7525
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'