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_7709174
_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 Fe N3 Si6, C43 H78 K2 N2 O4 P'
_chemical_formula_sum            'C61 H132 Fe K2 N5 O4 P Si6'
_chemical_formula_weight         1333.27
_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                 103.571(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9890(17)
_cell_length_b                   26.471(3)
_cell_length_c                   18.6846(19)
_cell_measurement_reflns_used    14385
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.36
_cell_volume                     8168.2(15)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1788
_diffrn_reflns_av_unetI/netI     0.1277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.360
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.8725
_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. = 0.780 (run 2)   max. = 1.615 (run 2)    spread = 0.8
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       needle
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         14385
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0754P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7852
_reflns_number_total             14385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03805b2.cif
_cod_data_source_block           2b_sidipppk2_fel3
_cod_depositor_comments
'Adding full bibliography for 7709171--7709174.cif.'
_cod_original_cell_volume        8168.0(15)
_cod_database_code               7709174
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.843
_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. Restrained distances
 H02H-H0AB
 -2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq,
Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C3AA(0.5) H3AA(0.5)
 H3AB(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
5.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00V(H00V), C01H(H01H), C01Q(H01Q)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C01I(H01G,H01I), C01N(H01J,H01K), C01P(H01O,H01P),
 C01T(H01X,H01Y), C01V(H01,H25), C022(H02G,H02H), C023(H02I,H02J), C3AA(H3AA,
 H3AB), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00Q(H00Q), C00X(H00X), C013(H013), C017(H017), C019(H019)
5.d Idealised Me refined as rotating group:
 C00T(H00A,H00B,H00C), C00U(H00D,H00E,H00F), C00Y(H00G,H00H,H00I), C010(H5,H,
 HA), C011(H6,HB,HC), C012(H7,HD,HE), C014(H8,HF,HG), C015(H9,HH,HI), C018(H10,
 HJ,HK), C01A(H11,HL,HM), C01B(H12,HN,HO), C01C(H13,HP,HQ), C01D(H14,HR,HS),
 C01E(H01A,H01B,H01C), C01F(H01D,H01E,H01F), C01G(H15,HT,HU), C01J(H16,HV,HW),
 C01K(H17,HX,HY), C01L(H18,HZ,H20), C01M(H19,H21,H22), C01O(H01L,H01M,H01N),
 C01R(H01R,H01S,H01T), C01S(H01U,H01V,H01W), C01U(H01Z,H23,H24), C01W(H1,H26,
 H27), C01X(H2,H28,H29), C01Y(H3,H30,H31), C01Z(H4,H32,H33), C020(H02A,H02B,
 H02C), C021(H02D,H02E,H02F), C024(H02K,H02L,H02M), C025(H02N,H02O,H02P),
 C026(H02Q,H02R,H02S), C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              762
_shelx_hkl_checksum              82977
_olex2_submission_special_instructions 'No special instructions were received'