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_7126736
_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_formula_moiety         'C38 H38 B2 Fe N2 P2'
_chemical_formula_sum            'C38 H38 B2 Fe N2 P2'
_chemical_formula_weight         662.11
_chemical_properties_physical    Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-03
_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                104.204(2)
_cell_angle_beta                 92.996(2)
_cell_angle_gamma                105.812(2)
_cell_formula_units_Z            4
_cell_length_a                   14.1841(8)
_cell_length_b                   14.9374(9)
_cell_length_c                   23.6074(14)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.362
_cell_measurement_theta_min      2.935
_cell_volume                     4627.2(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      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II CPAD'
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            149163
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0631 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.9053. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.950
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, tetrahydrofuran'
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.941
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         18967
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0953P)^2^+8.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15997
_reflns_number_total             18967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02152k2.cif
_cod_data_source_block           4-BH3
_cod_depositor_comments
;
Adding full bibliography for 7126735--7126738.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H76 B4 Fe2 N4 P4'
_cod_original_formula_weight         1324.22
_cod_original_formula_moiety         '2(C38 H38 B2 Fe N2 P2)'
_cod_original_formula_units_Z            2
_cod_database_code               7126736
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 B4-H4B
 1.15 with sigma of 0.02
 B2-H2D
 1.15 with sigma of 0.02
 B3-H3C
 1.15 with sigma of 0.02
 B2-H2E
 1.15 with sigma of 0.02
 B1-H1E
 1.15 with sigma of 0.02
 B3-H3B
 1.15 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C39(H39A,H39B), C40(H40A,H40B)
3.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), C42(H42), C43(H43), C44(H44),
  C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
  C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76)
;
_shelx_res_checksum              70117
_shelx_hkl_checksum              59956
_shelx_fab_checksum              6933
_olex2_submission_special_instructions 'No special instructions were received'