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_7708173
_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 Fe N5 O'
_chemical_formula_sum            'C35 H40 Cl Fe N5 O'
_chemical_formula_weight         638.02
_chemical_name_systematic        PhOPy(afaCy)2FeCl
_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
_audit_creation_date             2021-07-12
_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                107.625(2)
_cell_angle_beta                 99.068(2)
_cell_angle_gamma                106.032(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2743(3)
_cell_length_b                   14.0697(5)
_cell_length_c                   16.2126(6)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.59
_cell_volume                     1667.83(11)
_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      100.15
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  Mo_duo
_diffrn_measurement_method       '\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
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24340
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.413
_diffrn_reflns_theta_min         1.694
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0609 before and 0.0550 after correction. 
The Ratio of minimum to maximum transmission is 0.9052. 
The \l/2 correction factor is 0.00150. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_id                mo_dd68n
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0618P)^2^+0.6102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6772
_reflns_number_total             8309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02585f2.cif
_cod_data_source_block           dm30h_0m
_cod_database_code               7708173
_shelx_shelxl_version_number     2018/3
_audit_contact_letter
;
? 
;
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.028) H4(0.028) H15(0.022) H16(0.022) H29(0.02) H18(0.021)
 H13A(0.036) H13B(0.036) H13C(0.036) H30(0.022) H10(0.031) H26(0.023)
 H23A(0.027) H23B(0.027) H27(0.022) H24A(0.025) H24B(0.025) H8(0.031)
 H35A(0.026) H35B(0.026) H2(0.036) H19(0.021) H22A(0.027) H22B(0.027)
 H21A(0.028) H21B(0.028) H9(0.035) H34A(0.03) H34B(0.03) H31A(0.027)
 H31B(0.027) H33A(0.034) H33B(0.034) H20A(0.026) H20B(0.026) H32A(0.033)
 H32B(0.033) H5A(0.039) H3(0.051) H4A(0.054)
 Fixed X: H5(0.128618) H4(0.522233) H15(0.747698) H16(0.85771) H29(-0.159442)
 H18(0.795721) H13A(0.648937) H13B(0.470147) H13C(0.469328) H30(-0.213262)
 H10(0.677407) H26(0.172715) H23A(0.905051) H23B(0.696531) H27(-0.10085)
 H24A(0.896944) H24B(0.785166) H8(0.784176) H35A(-0.153222) H35B(0.017237)
 H2(0.395664) H19(0.526388) H22A(0.906801) H22B(0.797516) H21A(0.532435)
 H21B(0.646294) H9(0.80159) H34A(-0.333139) H34B(-0.216908) H31A(-0.020364)
 H31B(0.105627) H33A(-0.212281) H33B(-0.019836) H20A(0.526113) H20B(0.734907)
 H32A(-0.063002) H32B(-0.239429) H5A(0.85352) H3(0.585726) H4A(0.823791)
 Fixed Y: H5(0.286855) H4(0.397793) H15(0.818959) H16(0.741396) H29(0.337152)
 H18(0.549282) H13A(0.82214) H13B(0.784589) H13C(0.809917) H30(0.155207)
 H10(0.743276) H26(0.708102) H23A(0.331124) H23B(0.284765) H27(0.546534)
 H24A(0.411696) H24B(0.451117) H8(0.485425) H35A(0.142083) H35B(0.11432)
 H2(0.118538) H19(0.322853) H22A(0.219171) H22B(0.147848) H21A(0.136814)
 H21B(0.098552) H9(0.660097) H34A(-0.017952) H34B(-0.044532) H31A(0.138663)
 H31B(0.117069) H33A(-0.141626) H33B(-0.064045) H20A(0.21914) H20B(0.265928)
 H32A(-0.047373) H32B(-0.024113) H5A(0.366691) H3(0.062726) H4A(0.188911)
 Fixed Z: H5(0.719758) H4(0.565385) H15(0.804282) H16(0.672792) H29(0.731649)
 H18(0.56029) H13A(0.92743) H13B(0.954033) H13C(0.864193) H30(0.68851)
 H10(1.027731) H26(0.86993) H23A(0.335258) H23B(0.302902) H27(0.80735)
 H24A(0.484644) H24B(0.420517) H8(1.043379) H35A(0.547896) H35B(0.576974)
 H2(0.723516) H19(0.414355) H22A(0.41773) H22B(0.316053) H21A(0.355557)
 H21B(0.419692) H9(1.112069) H34A(0.554191) H34B(0.486032) H31A(0.802321)
 H31B(0.738703) H33A(0.583411) H33B(0.596339) H20A(0.505015) H20B(0.536893)
 H32A(0.738402) H32B(0.713115) H5A(0.965984) H3(0.802945) H4A(0.921077)
;
_shelx_res_checksum              44314
_shelx_fab_checksum              46467
_olex2_submission_original_sample_id dm30h
_olex2_submission_special_instructions 'No special instructions were received'