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_4349929
_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_absolute_configuration rmad
_chemical_formula_moiety         'C43 H58 Cl2 K Mn O6 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C45 H63 Cl2 K Mn O6.5 P'
_chemical_formula_weight         903.86
_chemical_name_systematic        K(18-C-6)MnCl2
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 106.264(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8360(2)
_cell_length_b                   17.5755(3)
_cell_length_c                   21.9420(4)
_cell_measurement_reflns_used    40795
_cell_measurement_temperature    179.9(3)
_cell_measurement_theta_max      30.7210
_cell_measurement_theta_min      3.1690
_cell_volume                     4752.00(15)
_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      179.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_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     -4.00  27.92   0.38    2.93    --   -1.60 -82.00 -30.00   84
  2  \w    -46.00   4.16   0.38    2.93    --   -1.60 -77.00-150.00  132
  3  \w    -46.00 -14.84   0.38    2.93    --   -1.60 -77.00  90.00   82
  4  \w    -21.00  21.18   0.38    2.93    --   -1.60 -82.00 120.00  111
  5  \w    -91.00 -34.00   0.38    2.93    --   -1.60 -38.00 -90.00  150
  6  \w    -27.00   0.36   0.38    2.93    --   -1.60 -38.00 -90.00   72
  7  \w    -61.00  10.06   0.38    2.93    --   -1.60 -57.00 -30.00  187
  8  \w    -45.00  22.26   0.38    2.93    --   -1.60 -77.00-120.00  177
  9  \w    -14.00  88.22   0.38    2.93    --    1.90  38.00-180.00  269
;
_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      -0.0251613000
_diffrn_orient_matrix_UB_12      0.0188258000
_diffrn_orient_matrix_UB_13      0.0207321000
_diffrn_orient_matrix_UB_21      -0.0186998000
_diffrn_orient_matrix_UB_22      0.0288480000
_diffrn_orient_matrix_UB_23      -0.0230665000
_diffrn_orient_matrix_UB_31      -0.0482675000
_diffrn_orient_matrix_UB_32      -0.0210237000
_diffrn_orient_matrix_UB_33      -0.0131525000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89653
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91268
_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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 9483 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         21681
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.9012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                20726
_reflns_number_total             21681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01054d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;

2020-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H126 Cl4 K2 Mn2 O13 P2'
_cod_original_formula_weight         1807.72
_cod_original_formula_moiety         '2(C43 H58 Cl2 K Mn O6 P), C4 H10 O'
_cod_original_formula_units_Z            2
_cod_database_code               4349929
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P Mn O N Si Cl'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.56
_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:
 C71(H71A,H71B), C79(H79A,H79B), C67(H67A,H67B), C73(H73A,H73B), C24(H24A,
 H24B), C85(H85A,H85B), C78(H78A,H78B), C81(H81A,H81B), C80(H80A,H80B),
 C30(H30A,H30B), C28(H28A,H28B), C26(H26A,H26B), C82(H82A,H82B), C69(H69A,H69B),
  C86(H86A,H86B), C36(H36A,H36B), C77(H77A,H77B), C75(H75A,H75B), C84(H84A,
 H84B), C37(H37A,H37B), C83(H83A,H83B), C38(H38A,H38B), C35(H35A,H35B),
 C42(H42A,H42B), C43(H43A,H43B), C32(H32A,H32B), C33(H33A,H33B), C76(H76A,H76B),
  C40(H40A,H40B), C41(H41A,H41B), C39(H39A,H39B), C34(H34A,H34B), C89(H89A,
 H89B), C88(H88A,H88B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C51(H51), C53(H53), C60(H60), C52(H52), C50(H50), C58(H58),
 C10(H10), C9(H9), C16(H16), C15(H15), C7(H7), C66(H66), C59(H59), C8(H8),
 C62(H62), C63(H63), C56(H56), C13(H13), C23(H23), C22(H22), C65(H65), C14(H14),
  C57(H57), C19(H19), C64(H64), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C74(H74A,H74B,H74C), C72(H72A,H72B,H72C), C68(H68A,H68B,
 H68C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C70(H70A,
 H70B,H70C), C87(H87A,H87B,H87C), C90(H90A,H90B,H90C)
;
_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.786