First-row early transition metal complexes with a highly sterically demanding triisopropylphenyl amino triphenolate ligand: synthesis and applications
Bae, Dae Young; Park, Gyeong Su; Ko, Nakeun; Son, Kyung-sun; Lee, Eunsung; Dalton Transactions  (2019) –; doi:10.1039/C9DT00456D

data_7049158
_publ_section_title
;
 First-row early transition metal complexes with a highly sterically
 demanding triisopropylphenyl amino triphenolate ligand: synthesis and
 applications
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00456D
_journal_year                    2019
_chemical_formula_moiety         'C75 H99.05 Mn N Na2 O6'
_chemical_formula_sum            'C75 H99.06 Mn N Na2 O6'
_chemical_formula_weight         1211.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.612(4)
_cell_length_b                   27.311(6)
_cell_length_c                   30.616(6)
_cell_measurement_reflns_used    60522
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.482
_cell_volume                     15562(6)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7000
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            60522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.482
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_description       plate
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         15909
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0682
_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^)+(0.1331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9297
_reflns_number_total             15909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00456d2.cif
_cod_data_source_block           pbca
_cod_original_cell_volume        15562(5)
_cod_database_code               7049158
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 C73, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C73, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C29A, C30, C31A, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=1-FVAR(1)
 Sof(H10)=Sof(H10A)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H57(0.5) H57A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C29(0.5) H29(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C29A(0.5) H29A(0.5) C31A(0.5) H31D(0.5)
 H31E(0.5) H31F(0.5) C58A(0.5) H58D(0.5) H58E(0.5) H58F(0.5)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C35(H35), C7(H7), C54(H54), C57(H57), C57(H57A), C10(H10),
 C10(H10A), C32(H32), C29(H29), C29A(H29A)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C44(H44A,H44B), C66(H66A,H66B), C75(H75A,H75B), C72(H72A,
 H72B), C73(H73A,H73B), C74(H74A,H74B)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C6(H6), C17(H17), C18(H18), C41(H41), C40(H40), C50(H50), C69(H69),
 C46(H46), C2(H2), C63(H63), C65(H65), C39(H39), C64(H64), C28(H28), C24(H24)
4.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C15(H15A,H15B,H15C), C67(H67A,H67B,H67C), C14(H14A,H14B,
 H14C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C52(H52A,
 H52B,H52C), C8(H8A,H8B,H8C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C9(H9A,
 H9B,H9C), C30(H30D,H30E,H30F), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C),
 C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C58(H58A,H58B,H58C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C31A(H31D,H31E,H31F), C58A(H58D,H58E,H58F),
 C53(H53A,H53B,H53C), C12A(H12D,H12E,H12F), C11A(H11D,H11E,H11F)
;
_shelx_res_checksum              85039
_shelx_hkl_checksum              79843
_shelx_fab_checksum              32606
_olex2_submission_special_instructions 'No special instructions were received'