Synthesis of a series of M(ii) (M = Mn, Fe, Co) chloride complexes with both inter- and intra-ligand hydrogen bonding interactions
Leahy, Clare A.; Drummond, Michael J.; Vura-Weis, Josh; Fout, Alison R.; Dalton Transactions  (2021) –; doi:10.1039/D1DT02585F

data_7708172
_publ_section_title
;
 Synthesis of a series of M(ii) (M = Mn, Fe, Co) chloride complexes with
 both inter- and intra-ligand hydrogen bonding interactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02585F
_journal_year                    2021
_chemical_formula_moiety         'C35 H40 Cl Mn N5 O'
_chemical_formula_sum            'C35 H40 Cl Mn N5 O'
_chemical_formula_weight         637.11
_chemical_name_systematic        PhOPy(afaCy)2MnCl
_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     iterative
_audit_creation_date             2021-07-15
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.8761(9)
_cell_angle_beta                 95.6991(9)
_cell_angle_gamma                92.0161(9)
_cell_formula_units_Z            2
_cell_length_a                   8.2117(2)
_cell_length_b                   13.3475(4)
_cell_length_c                   14.2019(4)
_cell_measurement_reflns_used    29380
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      50.804
_cell_measurement_theta_min      4.992
_cell_volume                     1528.34(7)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.9-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2014/7 
(Bruker, 2014) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  mo_dd68n_0m
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45633
_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         25.415
_diffrn_reflns_theta_min         2.496
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             670
_exptl_crystal_id                mo_dd68n_0m
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 1 1) scattering
planes roughly normal to the spindle axis. 
;
_exptl_crystal_recrystallization_method
'Suitable crystals were grown from a vapor diffusion of diethyl ether into aconcentrated solution in DCM.'
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0337P)^2^+0.9812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5063
_reflns_number_total             5609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02585f2.cif
_cod_data_source_block           mo_dd68n_0m
_cod_database_code               7708172
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.924
_exptl_absorpt_special_details
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  170
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
multiscan methods using SADABS v2016/2 (Bruker, 2012).  
No decay correction was applied.    
;
_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 H(H) groups, All C(H,H,H) groups 
2. Others 
 Sof(H29a)=Sof(N5A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31c)=Sof(H31d)= 
 Sof(C32A)=Sof(H32c)=Sof(H32d)=Sof(C33A)=Sof(H33c)=Sof(H33d)=Sof(C34A)= 
 Sof(H34c)=Sof(H34d)=Sof(C35A)=Sof(H35c)=Sof(H35d)=1-FVAR(1) 
 Sof(N5)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31a)=Sof(H31b)=Sof(C35)= 
 Sof(H35a)=Sof(H35b)=Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(C34)=Sof(H34a)=Sof(H34b)= 
 Sof(C32)=Sof(H32a)=Sof(H32b)=FVAR(1) 
 Sof(H19a)=Sof(C24A)=Sof(H24c)=Sof(H24d)=Sof(C23A)=Sof(H23c)=Sof(H23d)= 
 Sof(C22A)=Sof(H22c)=Sof(H22d)=Sof(C21A)=Sof(H21c)=Sof(H21d)=Sof(C20A)= 
 Sof(H20c)=Sof(H20d)=1-FVAR(2) 
 Sof(H19)=Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(C22)= 
 Sof(H22a)=Sof(H22b)=Sof(C20)=Sof(H20a)=Sof(H20b)=Sof(C21)=Sof(H21a)=Sof(H21b)= 
 FVAR(2) 
 Fixed U11: N4(0.016833) 
 Fixed U12: N4(-0.004128) 
 Fixed U13: N4(-0.002366) 
 Fixed U22: N4(0.016217) 
 Fixed U23: N4(-0.001506) 
 Fixed U33: N4(0.02078) 
3.a Ternary CH refined with riding coordinates: 
 C19(H19), C19(H19a), C30(H30), C30A(H30A) 
3.b Secondary CH2 refined with riding coordinates: 
 C31(H31a,H31b), C35(H35a,H35b), C33(H33a,H33b), C34(H34a,H34b), C32(H32a, 
 H32b), C23(H23a,H23b), C24(H24a,H24b), C22(H22a,H22b), C20(H20a,H20b), 
 C21(H21a,H21b), C31A(H31c,H31d), C32A(H32c,H32d), C33A(H33c,H33d), C34A(H34c, 
 H34d), C35A(H35c,H35d), C24A(H24c,H24d), C23A(H23c,H23d), C22A(H22c,H22d), 
 C21A(H21c,H21d), C20A(H20c,H20d) 
3.c Aromatic/amide H refined with riding coordinates: 
 C10(H10), C8(H8), C18(H18), C26(H26), C27(H27), C16(H16), C9(H9), C3(H3), 
 C15(H15), C5(H5a), C4(H4a), C2(H2), C29(H29), C29(H29a) 
3.d Idealised Me refined as rotating group: 
 C13(H13a,H13b,H13c) 
;
_shelx_res_checksum              72499
_shelx_hkl_checksum              16870
_olex2_date_sample_completion    2021-05-07
_olex2_date_sample_data_collection 2018-06-18
_olex2_date_sample_submission    2018-06-18
_olex2_exptl_crystal_mounting_method
;
0.3 mm cryo-loop (Hampton Research) with the (-3 1 1) scattering
planes roughly normal to the spindle axis.
;
_olex2_submission_original_sample_id dd68n
_olex2_submission_special_instructions 'No special instructions were received'