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_7709171
_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         'C54 H76 Mn N4 P2'
_chemical_formula_sum            'C54 H76 Mn N4 P2'
_chemical_formula_weight         898.06
_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             2021-09-30
_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                110.589(2)
_cell_angle_beta                 103.611(2)
_cell_angle_gamma                96.697(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7707(5)
_cell_length_b                   10.8284(6)
_cell_length_c                   12.2278(6)
_cell_measurement_reflns_used    4504
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.59
_cell_measurement_theta_min      2.29
_cell_volume                     1266.00(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22106
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.732
_diffrn_reflns_theta_min         2.289
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0851 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.9410. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             483
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.9774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3517
_reflns_number_total             4814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03805b2.cif
_cod_data_source_block           1_mn_psidipp2
_cod_depositor_comments
'Adding full bibliography for 7709171--7709174.cif.'
_cod_database_code               7709171
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.939
_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.a Ternary CH refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00J(H00J), C00O(H00O)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00C(H00C), C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M)
2.d Idealised Me refined as rotating group:
 C00N(H00B,H00D,H00E), C00P(H00H,H00N,H00P), C00Q(H00Q,H00R,H00S), C00R(H00T,
 H00U,H00V), C00S(H00W,H00X,H00Y), C00T(H00Z,H,HA), C00U(H00,HB,HC), C00V(H1,HD,
 HE)
;
_shelx_res_checksum              71159
_shelx_hkl_checksum              10300
_olex2_submission_special_instructions 'No special instructions were received'