<i>Z</i>-selective dimerization of terminal alkynes by a (PNNP)Fe<sup>II</sup> complex.
Stevens, Jeremiah E.; Miller, Justin D.; Fitzsimmons, Matthew C.; Moore, Curtis E.; Thomas, Christine M.; Chemical communications (Cambridge, England) 60 (2024) 5169–5172; doi:10.1039/d4cc00469h

data_7132974
_publ_section_title
;
 <i>Z</i>-selective dimerization of terminal alkynes by a
 (PNNP)Fe<sup>II</sup> complex.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5169
_journal_page_last               5172
_journal_paper_doi               10.1039/d4cc00469h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C54 H44 Fe N2 P2, 4(C6 H5 F)'
_chemical_formula_sum            'C78 H64 F4 Fe N2 P2'
_chemical_formula_weight         1223.10
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.2120(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.4666(15)
_cell_length_b                   13.8824(7)
_cell_length_c                   16.5411(7)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.32
_cell_volume                     6171.2(5)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2021)'
_computing_data_collection       'APEX3 v2021.10-0 (Bruker, 2021)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon III area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            152619
_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         26.398
_diffrn_reflns_theta_min         2.496
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1655 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.7221.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: fluorobenzene, methyltertbutyl ether'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0379P)^2^+4.9405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5348
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00469h2.cif
_cod_data_source_block           thomas_jes117_0m
_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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7132971--7132974.cif.
;
_cod_database_code               7132974
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(H1SB)=Sof(F2SB)=1-FVAR(1)
 Sof(H2SB)=Sof(F1SB)=FVAR(1)
 Sof(H1SA)=Sof(F2SA)=1-FVAR(2)
 Sof(H2SA)=Sof(F1SA)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C26(H26), C27(H27), C25(H25), C5(H5), C19(H19), C4(H4), C17(H17),
 C21(H21), C23(H23), C24(H24), C11(H11), C6(H6), C7(H7), C14(H14), C20(H20),
 C12(H12), C13(H13), C18(H18), C2SB(H2SB), C4SB(H4SB), C3SB(H3SB), C6SB(H6SB),
 C1SB(H1SB), C5SB(H5SB), C3SA(H3SA), C6SA(H6SA), C4SA(H4SA), C2SA(H2SA),
 C1SA(H1SA), C5SA(H5SA)
;
_shelx_res_checksum              80106
_shelx_hkl_checksum              36088
_olex2_submission_special_instructions 'No special instructions were received'