<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_7132972
_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         'C48 H50 Fe N4 P2'
_chemical_formula_sum            'C48 H50 Fe N4 P2'
_chemical_formula_weight         800.71
_chemical_properties_physical    Air-sensitive,Moisture-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   geom
_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                90.015(2)
_cell_angle_beta                 96.865(3)
_cell_angle_gamma                100.703(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7765(8)
_cell_length_b                   13.6127(9)
_cell_length_c                   14.6156(10)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.25
_cell_volume                     2091.1(3)
_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
_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 0.998
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            101157
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         1.938
_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    0.475
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0686 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.7436.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8545
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0391P)^2^+1.0320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7249
_reflns_number_total             8545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00469h2.cif
_cod_data_source_block           thomas_jes143_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               7132972
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.797
_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. Restrained distances
 C48-C46B \\sim C48-C46A
 with sigma of 0.02
 C48-C45B \\sim C48-C45A
 with sigma of 0.02
 C48-C47B \\sim C48-C47A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C45B) = Uanis(C45A)
4. Rigid body (RIGU) restrains
 C48, C46B, C45B, C47B, C47A, C46A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C45B)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C47B)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C41(H41), C18(H18), C12(H12), C34(H34), C24(H24), C44(H44),
 C30(H30), C17(H17), C32(H32), C25(H25), C28(H28), C37(H37), C19(H19), C31(H31),
  C22(H22), C29(H29), C36(H36), C26(H26), C42(H42), C38(H38), C23(H23),
 C20(H20), C10(H10), C35(H35), C16(H16), C11(H11), C13(H13)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C46B(H46A,H46B,H46C),
 C45B(H45A,H45B,H45C), C47B(H47A,H47B,H47C), C47A(H47D,H47E,H47F), C45A(H45D,
 H45E,H45F), C46A(H46D,H46E,H46F)
;
_shelx_res_checksum              93078
_shelx_hkl_checksum              39622
_olex2_submission_special_instructions 'No special instructions were received'