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_7708174
_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 Co N5 O, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C35.5 H41 Cl2 Co N5 O'
_chemical_formula_weight         683.56
_chemical_name_systematic        PhOPy(afaCy)2CoCl
_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             2021-07-21
_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                93.4590(10)
_cell_angle_beta                 91.0240(10)
_cell_angle_gamma                106.6890(10)
_cell_formula_units_Z            4
_cell_length_a                   12.8543(4)
_cell_length_b                   13.1875(4)
_cell_length_c                   21.8904(7)
_cell_measurement_reflns_used    84259
_cell_measurement_temperature    99.95
_cell_measurement_theta_max      50.826
_cell_measurement_theta_min      4.766
_cell_volume                     3545.59(19)
_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      99.95
_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 0.997
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Venture/Photon 100 Mo'
_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_dd29n
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            175399
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.425
_diffrn_reflns_theta_min         2.383
_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    0.669
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1432
_exptl_crystal_id                mo_dd29n
_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 0 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.992
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+6.2172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11707
_reflns_number_total             13068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02585f2.cif
_cod_data_source_block           mo_dd29n_0m
_cod_depositor_comments
;

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C71 H82 Cl4 Co2 N10 O2'
_cod_original_formula_weight         1367.12
_cod_original_formula_moiety         '2(C35 H40 Cl Co N5 O), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_database_code               7708174
_shelx_shelxl_version_number     2018/3
_audit_contact_letter
;
? 
;
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.768
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H53(0.022) H62(0.019) H61(0.018) H64(0.018) H26(0.023) H45(0.019)
 H10A(0.021) H65(0.021) H29(0.024) H27(0.024) H8(0.02) H5A(0.024) H43(0.021)
 H9A(0.023) H48A(0.026) H48B(0.026) H48C(0.026) H54(0.026) H44(0.021)
 H18(0.028) H51(0.025) H66A(0.027) H66B(0.027) H50(0.023) H4A(0.029) H70A(0.03)
 H70B(0.03) H19(0.029) H3(0.031) H2(0.029) H30(0.029) H35A(0.032) H35B(0.032)
 H15(0.032) H37(0.03) H13A(0.034) H13B(0.034) H13C(0.034) H33A(0.033)
 H33B(0.033) H16(0.036) H55A(0.033) H55B(0.033) H69A(0.035) H69B(0.035)
 H38(0.031) H40(0.031) H32A(0.039) H32B(0.039) H39(0.036) H67A(0.036)
 H67B(0.036) H56A(0.038) H56B(0.038) H31A(0.035) H31B(0.035) H34A(0.038)
 H34B(0.038) H59A(0.033) H59B(0.033) H20A(0.051) H20B(0.051) H68A(0.038)
 H68B(0.038) H58A(0.041) H58B(0.041) H57A(0.043) H57B(0.043) H21A(0.068)
 H21B(0.068) H24A(0.05) H24B(0.05) H23A(0.07) H23B(0.07) H22A(0.085)
 H22B(0.085) H71A(0.103) H71B(0.103) H10(0.129) H4(0.129) H9(0.129) H5(0.129)
 Fixed X: H53(0.464965) H62(1.17391) H61(1.10648) H64(0.97144) H26(0.782936)
 H45(0.981383) H10A(0.444329) H65(1.088608) H29(0.96346) H27(0.924875)
 H8(0.33082) H5A(0.307236) H43(0.88438) H9A(0.318947) H48A(1.027337)
 H48B(0.91031) H48C(0.951835) H54(0.37696) H44(0.975417) H18(0.626089)
 H51(0.557026) H66A(0.93972) H66B(1.019501) H50(0.744919) H4A(0.3044)
 H70A(1.228623) H70B(1.26862) H19(0.677193) H3(0.465714) H2(0.625067)
 H30(0.966973) H35A(1.003658) H35B(1.082124) H15(0.556366) H37(0.663875)
 H13A(0.65503) H13B(0.598772) H13C(0.527258) H33A(0.98784) H33B(1.052459)
 H16(0.565983) H55A(0.44013) H55B(0.517332) H69A(1.210564) H69B(1.290537)
 H38(0.64015) H40(0.779432) H32A(0.864837) H32B(0.941866) H39(0.699886)
 H67A(0.962005) H67B(1.002094) H56A(0.360095) H56B(0.284031) H31A(0.797999)
 H31B(0.826272) H34A(1.124916) H34B(1.149205) H59A(0.518131) H59B(0.441876)
 H20A(0.616573) H20B(0.737091) H68A(1.142657) H68B(1.132326) H58A(0.36085)
 H58B(0.284645) H57A(0.294006) H57B(0.424144) H21A(0.700083) H21B(0.66714)
 H24A(0.892282) H24B(0.858124) H23A(0.821329) H23B(0.941868) H22A(0.841508)
 H22B(0.88034) H71A(0.905365) H71B(0.848673)
 Fixed Y: H53(0.650845) H62(0.943682) H61(0.82391) H64(0.845775) H26(0.566213)
 H45(0.485807) H10A(0.443593) H65(1.075581) H29(0.610944) H27(0.653016)
 H8(0.396552) H5A(0.27923) H43(0.32257) H9A(0.460201) H48A(0.645411)
 H48B(0.583977) H48C(0.710861) H54(0.671474) H44(0.33975) H18(-0.050174)
 H51(0.622104) H66A(0.928653) H66B(0.860066) H50(0.618409) H4A(0.22332)
 H70A(0.948203) H70B(1.066872) H19(-0.122161) H3(0.211436) H2(0.251912)
 H30(0.476121) H35A(0.693574) H35B(0.623292) H15(0.194645) H37(0.554693)
 H13A(0.395911) H13B(0.478691) H13C(0.360126) H33A(0.734723) H33B(0.682422)
 H16(0.018116) H55A(0.576818) H55B(0.684446) H69A(1.133902) H69B(1.065727)
 H38(0.39446) H40(0.291303) H32A(0.583495) H32B(0.511948) H39(0.261184)
 H67A(0.927588) H67B(1.046002) H56A(0.628226) H56B(0.622343) H31A(0.480062)
 H31B(0.604308) H34A(0.605861) H34B(0.729642) H59A(0.86372) H59B(0.856802)
 H20A(-0.043666) H20B(0.031063) H68A(0.920715) H68B(1.023084) H58A(0.908056)
 H58B(0.799558) H57A(0.77983) H57B(0.814212) H21A(-0.111965) H21B(-0.195497)
 H24A(0.01449) H24B(-0.069398) H23A(-0.212754) H23B(-0.138345) H22A(-0.187056)
 H22B(-0.060902) H71A(0.29161) H71B(0.226595)
 Fixed Z: H53(1.090558) H62(1.07226) H61(1.157634) H64(0.935854) H26(0.334288)
 H45(1.141964) H10A(0.358331) H65(0.883886) H29(0.527761) H27(0.416219)
 H8(0.528206) H5A(0.587484) H43(0.979065) H9A(0.432287) H48A(1.18614)
 H48B(1.209608) H48C(1.216409) H54(1.000015) H44(1.073194) H18(0.405366)
 H51(1.194701) H66A(0.854707) H66B(0.83417) H50(1.225917) H4A(0.686006)
 H70A(0.851459) H70B(0.882373) H19(0.490301) H3(0.732572) H2(0.680046)
 H30(0.645942) H35A(0.622462) H35B(0.602666) H15(0.273284) H37(0.827198)
 H13A(0.277728) H13B(0.308885) H13C(0.288738) H33A(0.741758) H33B(0.787887)
 H16(0.305577) H55A(0.922259) H55B(0.89854) H69A(0.79426) H69B(0.773638)
 H38(0.772109) H40(0.912731) H32A(0.77702) H32B(0.757193) H39(0.815466)
 H67A(0.746097) H67B(0.777183) H56A(0.834299) H56B(0.891924) H31A(0.68354)
 H31B(0.673316) H34A(0.706772) H34B(0.696588) H59A(0.958442) H59B(1.016076)
 H20A(0.575848) H20B(0.592817) H68A(0.740264) H68B(0.707608) H58A(0.928346)
 H58B(0.951608) H57A(0.84431) H57B(0.849328) H21A(0.656) H21B(0.597702)
 H24A(0.51907) H24B(0.460906) H23A(0.524487) H23B(0.541806) H22A(0.632117)
 H22B(0.628489) H71A(0.695975) H71B(0.634072)
;
_smtbx_masks_special_details
;
A total of 83 electrons were masked in each asymmetric unit. 
This corresponds to one dichloromethane solvent molecule 
and one diethyl ether solvent molecule per asymmetric unit. 
;
_shelx_res_checksum              64958
_shelx_fab_checksum              68982
_olex2_date_sample_data_collection 2018-06-11
_olex2_date_sample_submission    2018-06-06
_olex2_submission_original_sample_id dd29n
_olex2_submission_special_instructions 'No special instructions were received'