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_7126737
_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         'C50 H58 B2 Fe N2 O4 P2'
_chemical_formula_sum            'C50 H58 B2 Fe N2 O4 P2'
_chemical_formula_weight         890.39
_chemical_properties_physical    Air-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             2020-02-06
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2020-03-18 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                83.392(2)
_cell_angle_beta                 73.967(2)
_cell_angle_gamma                72.760(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7019(8)
_cell_length_b                   14.3131(10)
_cell_length_c                   19.1169(14)
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    200
_cell_measurement_theta_max      24.085
_cell_measurement_theta_min      2.219
_cell_volume                     2937.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_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)'
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_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa APEX II Mo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82284
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_min         1.109
_diffrn_source                   'sealed tube'
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_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.7454
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0632 before and 0.0583 after correction. The Ratio of minimum to maximum transmission is 0.9157. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, tetrahydrofuran'
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_exptl_crystal_size_min          0.215
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0781
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+2.3883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8936
_reflns_number_total             12080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02152k2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126735--7126738.cif.
;
_cod_database_code               7126737
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.868
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.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)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              37528
_shelx_hkl_checksum              54582
_shelx_fab_checksum              17918
_olex2_submission_special_instructions 'No special instructions were received'