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_4349933
_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 Mn P2'
_chemical_formula_sum            'C62 H68 Mn P2'
_chemical_formula_weight         930.04
_chemical_name_systematic        Mn(L1)2
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5013(2)
_cell_length_b                   13.5013(2)
_cell_length_c                   27.8106(10)
_cell_measurement_reflns_used    18888
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.2070
_cell_measurement_theta_min      3.9690
_cell_volume                     5069.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -89.00  -4.00   0.50    7.87    --   -1.60 -57.00  60.00  170
  2  \w    -33.00   2.00   0.50    7.87    --   -1.60 -82.00   0.00   70
  3  \w    -88.00   6.00   0.50    7.87    --    1.90 -38.00 120.00  188
  4  \w     -6.00  80.00   0.50    7.87    --    1.90  38.00  30.00  172
  5  \w    -46.00 -11.00   0.50    7.87    --    1.90 -77.00 -90.00   70
  6  \w     -7.00  27.00   0.50    7.87    --    1.90 -77.00 -90.00   68
  7  \w    -32.00  14.00   0.50    7.87    --    1.90 -77.00-150.00   92
;
_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      -0.0217810000
_diffrn_orient_matrix_UB_12      -0.0450588000
_diffrn_orient_matrix_UB_13      0.0077427000
_diffrn_orient_matrix_UB_21      -0.0418783000
_diffrn_orient_matrix_UB_22      0.0264416000
_diffrn_orient_matrix_UB_23      0.0084868000
_diffrn_orient_matrix_UB_31      -0.0230740000
_diffrn_orient_matrix_UB_32      -0.0054788000
_diffrn_orient_matrix_UB_33      -0.0227723000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            72701
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_preparation       'MnCl2 + 2L1K'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 2101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0561P)^2^+1.8963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4849
_reflns_number_total             4987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01054d2.cif
_cod_data_source_block           exp_827
_cod_database_code               4349933
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Mg Mn P N Cl'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 99.47
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C30(H30A,H30B), C26(H26A,H26B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C10(H10), C9(H9), C17(H17), C19(H19), C13(H13), C14(H14),
 C15(H15), C16(H16), C23(H23), C21(H21), C20(H20), C22(H22)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              30119
_shelx_hkl_checksum              81585
_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 2.163
_oxdiff_exptl_absorpt_empirical_full_min 0.777