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_7709173
_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, C43 H78 K2 N2 O4 P'
_chemical_formula_sum            'C61 H132 K2 Mn N5 O4 P Si6'
_chemical_formula_weight         1332.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2021-09-30 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.993(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9431(12)
_cell_length_b                   26.5429(14)
_cell_length_c                   18.8061(13)
_cell_measurement_reflns_used    14522
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.35
_cell_volume                     8240.9(9)
_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_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.350
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9163
_exptl_absorpt_correction_T_min  0.7604
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Area X-Red 1.63.4.0 (STOE, 2017) Statistics over combined scale factors for x file reflections:
       min. = -0.218 (run 1)   max. = 1.724 (run 1)    spread = 1.9
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             2908
_exptl_crystal_size_max          0.747
_exptl_crystal_size_mid          0.695
_exptl_crystal_size_min          0.392
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         14522
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9138
_reflns_number_total             14522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03805b2.cif
_cod_data_source_block           2a_sidipppk2_mnl3
_cod_depositor_comments
'Adding full bibliography for 7709171--7709174.cif.'
_cod_database_code               7709173
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.750
_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. Uiso/Uaniso restraints and constraints
Uanis(C1AA) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) C1A(0.5) H1AC(0.5) H1AD(0.5) H1AE(0.5)
4.a Ternary CH refined with riding coordinates:
 C00N(H00N), C012(H012), C01B(H01F), C01U(H01Z)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C014(H01A,H01B), C019(H01C,H01D), C01J(H01N,H01O),
 C01O(H01S,H01T), C01P(H01U,H01V), C022(H02G,H02H), C023(H02I,H02J), C1AA(H1AA,
 H1AB), C2A(H2AA,H2AB)
4.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00Y(H00Y), C011(H011), C01A(H01E), C01I(H01M)
4.d Idealised Me refined as rotating group:
 C00M(H00D,H00E,H00F), C00T(H00G,H00H,H00I), C00V(H00A,H00B,H00C), C00W(H00J,
 H00K,H00L), C013(H5,H,HA), C015(H6,HB,HC), C016(H7,HD,HE), C017(H8,HF,HG),
 C018(H9,HH,HI), C01C(H10,HJ,HK), C01D(H11,HL,HM), C01E(H12,HN,HO), C01F(H01G,
 H01H,H01I), C01G(H01J,H01K,H01L), C01H(H13,HP,HQ), C01K(H01P,H01Q,H01R),
 C01L(H14,HR,HS), C01M(H15,HT,HU), C01N(H16,HV,HW), C01Q(H17,HX,HY), C01R(H18,
 HZ,H20), C01S(H19,H21,H22), C01T(H01W,H01X,H01Y), C01V(H01,H23,H24), C01W(H1,
 H25,H26), C01X(H2,H27,H28), C01Y(H3,H29,H30), C01Z(H4,H31,H32), C020(H02A,H02B,
 H02C), C021(H02D,H02E,H02F), C024(H02K,H02L,H02M), C025(H02N,H02O,H02P),
 C026(H02Q,H02R,H02S), C0AA(H0AA,H0AB,H0AC), C1A(H1AC,H1AD,H1AE)
;
_shelx_res_checksum              57725
_shelx_hkl_checksum              40943
_olex2_submission_special_instructions 'No special instructions were received'