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_4349931
_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         'C31 H36 Mn N P'
_chemical_formula_sum            'C31 H36 Mn N P'
_chemical_formula_weight         508.52
_chemical_name_systematic        L1MnNH2
_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             2018-08-18
_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                116.797(3)
_cell_angle_beta                 96.699(3)
_cell_angle_gamma                106.485(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0194(3)
_cell_length_b                   12.4401(4)
_cell_length_c                   13.4146(4)
_cell_measurement_reflns_used    12251
_cell_measurement_temperature    179.99(11)
_cell_measurement_theta_max      30.2810
_cell_measurement_theta_min      3.6370
_cell_volume                     1371.44(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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(11)
_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    -21.00  87.00   0.50    3.00    --   -1.60  38.00  30.00  216
  2  \w    -26.00  59.00   0.50    3.00    --   -1.60  19.00-120.00  170
  3  \w     35.00  66.00   0.50    3.00    --   -1.60  57.00 120.00   62
  4  \w    -25.00  53.00   0.50    3.00    --   -1.60  57.00 -30.00  156
  5  \w    -25.00   4.00   0.50    3.00    --   -1.60  57.00 120.00   58
  6  \w    -21.00  87.00   0.50    3.00    --   -1.60  38.00 -90.00  216
  7  \w    -24.00  16.00   0.50    3.00    --   -1.60  19.00 120.00   80
  8  \w     21.00  81.00   0.50    3.00    --   -1.60  19.00 120.00  120
  9  \w    -19.00  32.00   0.50    3.00    --    1.90 -77.00 -90.00  102
 10  \w      2.00  34.00   0.50    3.00    --    1.90 -82.00-150.00   64
 11  \w    -28.00  -1.00   0.50    3.00    --    1.90 -82.00-150.00   54
 12  \w      9.00  34.00   0.50    3.00    --    1.90 -82.00  90.00   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      0.0256712000
_diffrn_orient_matrix_UB_12      0.0634060000
_diffrn_orient_matrix_UB_13      0.0496466000
_diffrn_orient_matrix_UB_21      0.0661885000
_diffrn_orient_matrix_UB_22      -0.0061351000
_diffrn_orient_matrix_UB_23      0.0162440000
_diffrn_orient_matrix_UB_31      0.0299205000
_diffrn_orient_matrix_UB_32      0.0266167000
_diffrn_orient_matrix_UB_33      -0.0330504000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35623
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
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    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             538
_exptl_crystal_preparation       'L1MnCl + NaNH2'
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0902P)^2^+0.6933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5406
_reflns_number_total             6266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01054d2.cif
_cod_data_source_block           exp_1497
_cod_original_cell_volume        1371.44(8)
_cod_database_code               4349931
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P Mn Na N'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.994
_reflns_odcompleteness_completeness 99.75
_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), C26(H26A,H26B), C30(H30A,H30B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C17(H17), C11(H11), C10(H10), C9(H9), C19(H19), C14(H14),
 C15(H15), C16(H16), C23(H23), C20(H20), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              88277
_shelx_hkl_checksum              47439
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.746