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_4349928
_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         'C62 H68 Cl2 Mn2 P2'
_chemical_formula_sum            'C62 H68 Cl2 Mn2 P2'
_chemical_formula_weight         1055.88
_chemical_name_systematic        L1MnCl
_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             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                90
_cell_angle_beta                 98.822(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7602(2)
_cell_length_b                   14.8229(2)
_cell_length_c                   15.1688(2)
_cell_measurement_reflns_used    27339
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.8530
_cell_measurement_theta_min      2.3750
_cell_volume                     2835.13(7)
_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_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -46.00   8.00   0.50    1.95    --   -0.10 -77.00-180.00  108
  2  \w    -33.00  31.00   0.50    1.95    --   -0.10 -82.00  60.00  128
  3  \w    -24.00  31.00   0.50    1.95    --   -0.10  19.00-120.00  110
  4  \w     35.00  89.00   0.50    1.95    --   -0.10  19.00-120.00  108
  5  \w    -90.00 -26.00   0.50    1.95    --   -0.10 -57.00 -30.00  128
  6  \w    -13.00  19.00   0.50    1.95    --   -0.10 -57.00-180.00   64
  7  \w    -58.00 -33.00   0.50    1.95    --   -0.10 -38.00  60.00   50
  8  \w    -11.00  17.00   0.50    1.95    --   -0.10 -38.00  60.00   56
  9  \w    -66.00 -40.00   0.50    1.95    --   -0.10 -19.00 -90.00   52
 10  \w    -10.00  15.00   0.50    1.95    --   -0.10 -77.00 -60.00   50
 11  \w    -16.00   9.00   0.50    1.95    --   -0.10 -38.00 -90.00   50
 12  \w    -20.00   6.00   0.50    1.95    --   -0.10  19.00 150.00   52
 13  \w      5.00  30.00   0.50    1.95    --   -0.10 -82.00  30.00   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      -0.0399595000
_diffrn_orient_matrix_UB_12      0.0328789000
_diffrn_orient_matrix_UB_13      -0.0123335000
_diffrn_orient_matrix_UB_21      -0.0309985000
_diffrn_orient_matrix_UB_22      -0.0324269000
_diffrn_orient_matrix_UB_23      -0.0267688000
_diffrn_orient_matrix_UB_31      -0.0246711000
_diffrn_orient_matrix_UB_32      -0.0124793000
_diffrn_orient_matrix_UB_33      0.0370244000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.945
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81516
_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 reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0809P)^2^+3.2912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5849
_reflns_number_total             6497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01054d2.cif
_cod_data_source_block           exp_863
_cod_database_code               4349928
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O P Mn Si Cl '
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.987
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C8(H8), C9(H9), C23(H23), C13(H13), C17(H17), C16(H16),
 C15(H15), C19(H19), C14(H14), C21(H21), C22(H22), C20(H20)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C27(H27A,H27B,
 H27C)
;
_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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.619