Synthesis of the open-shell 3d-transition metal(II) bis(phosphinidenide) [Mn{P(sIDipp)}<sub>2</sub>].
Weller, Ruth; Balmer, Markus; Hänisch, Carsten von; Gunnar Werncke, C.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1765–1768; doi:10.1039/d1dt03805b

data_7709172
_publ_section_title
;
 Synthesis of the open-shell 3d-transition metal(II) bis(phosphinidenide)
 [Mn{P(sIDipp)}<sub>2</sub>].
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1765
_journal_page_last               1768
_journal_paper_doi               10.1039/d1dt03805b
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C18 H54 Mn N3 Si6, C18 H36 K N2 O6'
_chemical_formula_sum            'C36 H90 K Mn N5 O6 Si6'
_chemical_formula_weight         951.70
_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
_audit_creation_date             2021-10-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-13 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                84.190(6)
_cell_angle_beta                 77.760(6)
_cell_angle_gamma                89.530(6)
_cell_formula_units_Z            2
_cell_length_a                   11.4888(9)
_cell_length_b                   15.4353(12)
_cell_length_c                   16.6387(12)
_cell_measurement_reflns_used    12109
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.734
_cell_measurement_theta_min      2.418
_cell_volume                     2868.4(4)
_computing_cell_refinement       'X-Area Recipe 1.36.0.0 (STOE, 2020)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction        'X-Area X-Red 1.65.2.0 (STOE, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29082
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.734
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9567
_exptl_absorpt_correction_T_min  0.7904
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
X-Area LANA 1.83.8.0 (STOE, 2020) Statistics over combined scale factors for x file reflections:
       min. = 0.889 (run 1)   max. = 1.076 (run 2)    spread = 0.2
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.16
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         12109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9252
_reflns_number_total             12109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03805b2.cif
_cod_data_source_block           kcrypt222_mnl3
_cod_depositor_comments
;
Adding full bibliography for 7709171--7709174.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H180 K2 Mn2 N10 O12 Si12'
_cod_original_formula_weight         1903.41
_cod_original_formula_moiety         '2(C18 H54 Mn N3 Si6), 2(C18 H36 K N2 O6)'
_cod_original_formula_units_Z            1
_cod_database_code               7709172
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00K(H00V,H00W), C00L(H00X,H00Y), C00M(H00Z,H), C00N(H00,HA), C00O(H1,HB),
 C00R(H2,HC), C00W(H3,HD), C00X(H4,HE), C00Y(H5,HF), C013(H6,HG), C014(H7,HH),
 C015(H8,HI), C016(H9,HJ), C019(H10,HK), C01B(H11,HL), C01C(H12,HM), C01D(H13,
 HN), C01F(H14,HO)
2.b Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00Q(H00D,H00E,H00F), C00S(H00G,H00H,H00I), C00T(H00J,
 H00K,H00L), C00U(H00M,H00N,H00O), C00V(H00P,H00Q,H00R), C00Z(H00S,H00T,H00U),
 C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,H01H,H01I), C017(H01J,
 H01K,H01L), C018(H01M,H01N,H01O), C01A(H01P,H01Q,H01R), C01E(H01S,H01T,H01U),
 C01G(H01V,H01W,H01X), C01H(H01Y,HP,HQ), C01I(H01Z,HR,HS), C01J(H01,HT,HU)
;
_shelx_res_checksum              82466
_shelx_hkl_checksum              46667
_shelx_fab_checksum              57596
_olex2_submission_special_instructions 'No special instructions were received'