Metal-ligand cooperativity across two sites of a square planar iron(ii) complex ligated by a tetradentate PNNP ligand.
Hatzis, Gregory P.; Thomas, Christine M.; Chemical communications (Cambridge, England) 56 (2020) 8611–8614; doi:10.1039/d0cc02152k

data_7126738
_publ_section_title
;
 Metal-ligand cooperativity across two sites of a square planar iron(ii)
 complex ligated by a tetradentate PNNP ligand.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8611
_journal_page_last               8614
_journal_paper_doi               10.1039/d0cc02152k
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H41 Fe N2 P3, 1(C6 H6)'
_chemical_formula_sum            'C47 H47 Fe N2 P3'
_chemical_formula_weight         788.62
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-18 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.046(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3592(13)
_cell_length_b                   16.4666(12)
_cell_length_c                   14.4482(11)
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.788
_cell_measurement_theta_min      2.768
_cell_volume                     3969.1(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  MoSource_OSU
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            110238
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.787
_diffrn_reflns_theta_min         2.759
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0653 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.9176. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, benzene'
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 7197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         16891
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0458P)^2^+5.4590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                15698
_reflns_number_total             16891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02152k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7126735--7126738.cif.'
_cod_database_code               7126738
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.800
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.629(17)
 0.371(17)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C90A) = Uanis(C90) = Uanis(C89) = Uanis(C89A) = Uanis(C94) = Uanis(C94A)
= Uanis(C93) = Uanis(C93A) = Uanis(C92A) = Uanis(C92) = Uanis(C91A) = Uanis(C91)
Uanis(C88A) = Uanis(C85) = Uanis(C83A) = Uanis(C84A) = Uanis(C86) = Uanis(C87)
= Uanis(C85A) = Uanis(C88) = Uanis(C86A) = Uanis(C83) = Uanis(C84) = Uanis(C87A)
4. Others
 Sof(C91A)=Sof(H91A)=Sof(C90A)=Sof(H90A)=Sof(C89A)=Sof(H89A)=Sof(C94A)=
 Sof(H94A)=Sof(C93A)=Sof(H93A)=Sof(C92A)=Sof(H92A)=1-FVAR(1)
 Sof(C89)=Sof(H89)=Sof(C94)=Sof(H94)=Sof(C93)=Sof(H93)=Sof(C92)=Sof(H92)=
 Sof(C91)=Sof(H91)=Sof(C90)=Sof(H90)=FVAR(1)
 Sof(C88A)=Sof(H88A)=Sof(C87A)=Sof(H87A)=Sof(C86A)=Sof(H86A)=Sof(C85A)=
 Sof(H85A)=Sof(C84A)=Sof(H84A)=Sof(C83A)=Sof(H83A)=1-FVAR(2)
 Sof(C85)=Sof(H85)=Sof(C84)=Sof(H84)=Sof(C83)=Sof(H83)=Sof(C88)=Sof(H88)=
 Sof(C87)=Sof(H87)=Sof(C86)=Sof(H86)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C42(H42A,H42B), C43(H43A,H43B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C45(H45), C46(H46), C47(H47),
  C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C75(H75), C76(H76),
 C77(H77), C78(H78), C79(H79), C85(H85), C84(H84), C83(H83), C88(H88), C87(H87),
  C86(H86), C89(H89), C94(H94), C93(H93), C92(H92), C91(H91), C90(H90),
 C88A(H88A), C87A(H87A), C86A(H86A), C85A(H85A), C84A(H84A), C83A(H83A),
 C91A(H91A), C90A(H90A), C89A(H89A), C94A(H94A), C93A(H93A), C92A(H92A)
5.c Fitted hexagon refined as free rotating group:
 C85(C84,C83,C88,C87,C86), C89(C94,C93,C92,C91,C90), C88A(C87A,C86A,C85A,C84A,
 C83A), C91A(C90A,C89A,C94A,C93A,C92A)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C)
;
_shelx_res_checksum              69141
_shelx_hkl_checksum              20991
_olex2_submission_special_instructions 'No special instructions were received'