Synthesis and characterization of manganese(ii) complexes supported by cyclopentadienyl-phosphine ligands
Wang, Gao-Xiang; Yin, Jianhao; Li, Jiapeng; Yin, Zhu-Bao; Zhang, Wen-Xiong; Xi, Zhenfeng; Inorganic Chemistry Frontiers 6 (2019) 428–; doi:10.1039/C8QI01054D

data_4349930
_publ_section_title
;
 Synthesis and characterization of manganese(ii) complexes supported by
 cyclopentadienyl-phosphine ligands
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              428
_journal_paper_doi               10.1039/C8QI01054D
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C64 H74 Mn2 P2'
_chemical_formula_sum            'C64 H74 Mn2 P2'
_chemical_formula_weight         1015.05
_chemical_name_systematic        L1MnMe
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-01 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                70.396(4)
_cell_angle_beta                 88.916(3)
_cell_angle_gamma                62.000(5)
_cell_formula_units_Z            2
_cell_length_a                   12.9652(5)
_cell_length_b                   13.7431(7)
_cell_length_c                   19.5176(7)
_cell_measurement_reflns_used    18237
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.7810
_cell_measurement_theta_min      3.1380
_cell_volume                     2852.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  23.00   0.50    3.25    --   -1.60 -82.00 -90.00  112
  2  \w    -28.00  30.00   0.50    3.25    --   -1.60 -82.00  60.00  116
  3  \w    -39.00  29.00   0.50    3.25    --   -1.60 -77.00-150.00  136
  4  \w    -41.00  28.00   0.50    3.25    --   -1.60 -77.00 120.00  138
  5  \w    -32.00  28.00   0.50    3.25    --   -1.60 -82.00   0.00  120
  6  \w    -29.00   2.00   0.50    3.25    --   -1.60 -82.00  90.00   62
  7  \w    -22.00  31.00   0.50    3.25    --   -1.60 -82.00 -30.00  106
  8  \w    -26.00  -1.00   0.50    3.25    --    1.90 -82.00  60.00   50
  9  \w     60.00  88.00   0.50    3.25    --    1.90  57.00  90.00   56
 10  \w     24.00  69.00   0.50    3.25    --    1.90  57.00 150.00   90
 11  \w     64.00  89.00   0.50    3.25    --    1.90  38.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0227457000
_diffrn_orient_matrix_UB_12      0.0331954000
_diffrn_orient_matrix_UB_13      0.0086212000
_diffrn_orient_matrix_UB_21      0.0289811000
_diffrn_orient_matrix_UB_22      -0.0463356000
_diffrn_orient_matrix_UB_23      0.0348174000
_diffrn_orient_matrix_UB_31      0.0509071000
_diffrn_orient_matrix_UB_32      -0.0266432000
_diffrn_orient_matrix_UB_33      -0.0156256000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52369
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         11161
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0660P)^2^+1.1394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9140
_reflns_number_total             11161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01054d2.cif
_cod_data_source_block           4
_cod_original_cell_volume        2852.2(2)
_cod_database_code               4349930
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Mn P N Mg Cl'
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.989
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2C-C2
 1 with sigma of 0.02
 C2-H2A
 1 with sigma of 0.02
 C2-H2B
 1 with sigma of 0.02
 C1-H1C
 1 with sigma of 0.02
 C1-H1B
 1 with sigma of 0.02
 C1-H1A
 1 with sigma of 0.02
 H2A-H2B
 1.57 with sigma of 0.04
 H2A-H2C
 1.57 with sigma of 0.04
 H2B-H2C
 1.57 with sigma of 0.04
 H1C-H1A
 1.57 with sigma of 0.04
 H1A-H1B
 1.57 with sigma of 0.04
 H1C-H1B
 1.57 with sigma of 0.04
3. Rigid bond restraints
 Mn2, C2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Mn2, C1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C1, Mn1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C2, Mn1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Mn1, P1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 P2, Mn2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(H57C)=Sof(H57D)=Sof(C58B)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(1)
 Sof(H57A)=Sof(H57B)=Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C32(H32A,H32B), C28(H28A,H28B), C63(H63A,H63B), C30(H30A,
 H30B), C59(H59A,H59B), C61(H61A,H61B), C57(H57A,H57B), C57(H57C,H57D)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C15(H15), C43(H43), C21(H21), C25(H25), C19(H19),
 C42(H42), C46(H46), C9(H9), C40(H40), C17(H17), C41(H41), C50(H50), C16(H16),
 C18(H18), C52(H52), C56(H56), C10(H10), C22(H22), C54(H54), C49(H49), C53(H53),
  C23(H23), C55(H55), C48(H48), C47(H47), C24(H24)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C64(H64A,H64B,
 H64C), C33(H33A,H33B,H33C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C58A(H58A,H58B,H58C), C58B(H58D,H58E,H58F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.770