Synthesis and characterization of manganese triple-decker complexes.
Heinl, Sebastian; Balázs, Gábor; Bodensteiner, Michael; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1962–1966; doi:10.1039/c5dt01750e

data_7035322
_publ_section_title
;
 Synthesis and characterization of manganese triple-decker complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1962
_journal_page_last               1966
_journal_paper_doi               10.1039/c5dt01750e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C110 H130 Mn2 P4.7, 6 (C7 H8)'
_chemical_formula_sum            'C152 H178 Mn2 P4.7'
_chemical_formula_weight         2260.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-09 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.9973(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.11800(15)
_cell_length_b                   23.57334(16)
_cell_length_c                   17.22285(14)
_cell_measurement_reflns_used    29963
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.56
_cell_measurement_theta_min      3.29
_cell_volume                     6488.42(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.23t (Agilent, 2014)'
_computing_data_collection       'CrysAlisPro 1.171.38.23t (Agilent, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.23t (Agilent, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.0(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61294
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         73.611
_diffrn_reflns_theta_min         3.327
_exptl_absorpt_coefficient_mu    2.503
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.23t (Agilent, 2014)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             2421
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13251
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1237P)^2^+3.9321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12310
_reflns_number_total             13251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01750e2.cif
_cod_data_source_block           sh398_sq_mb
_cod_depositor_comments
'Adding full bibliography for 7035321--7035322.cif.'
_cod_original_cell_volume        6488.41(10)
_cod_database_code               7035322
_shelxl_version_number           2014/6
_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, All C(H,H,H,H,H,
  H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C42 \\sim C43A \\sim C43B: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02
C52 \\sim C53A \\sim C53B \\sim C53C \\sim C54A \\sim C54B \\sim C54C \\sim
C55A \\sim C55B \\sim C55C: within 2A with sigma of 0.03 and sigma for terminal
atoms of 0.03
3. Others
 Fixed Sof: P3(0.35) P4(0.35) P5(0.35) P8(0.15) P7(0.15) H32A(0.7) H32B(0.7)
 H32C(0.3) H32D(0.3) C33A(0.7) H33A(0.7) H33B(0.7) C33B(0.3) H33C(0.3)
 H33D(0.3) C34A(0.7) H34A(0.7) H34B(0.7) C34B(0.3) H34C(0.3) H34D(0.3)
 C35A(0.7) H35A(0.7) H35B(0.7) H35C(0.7) C35B(0.3) H35D(0.3) H35E(0.3)
 H35F(0.3) H42A(0.62) H42B(0.62) H42C(0.38) H42D(0.38) C43A(0.62) H43A(0.62)
 H43B(0.62) C43B(0.38) H43C(0.38) H43D(0.38) C44A(0.62) H44A(0.62) H44B(0.62)
 C44B(0.38) H44C(0.38) H44D(0.38) C45A(0.62) H45A(0.62) H45B(0.62) H45C(0.62)
 C45B(0.38) H45D(0.38) H45E(0.38) H45F(0.38) H52A(0.43) H52B(0.43) H52E(0.25)
 H52F(0.25) H52C(0.32) H52D(0.32) C53A(0.43) H53A(0.43) H53B(0.43) C53B(0.32)
 H53C(0.32) H53D(0.32) C53C(0.25) H53E(0.25) H53F(0.25) C54A(0.43) H54A(0.43)
 H54B(0.43) C54B(0.32) H54C(0.32) H54D(0.32) C54C(0.25) H54E(0.25) H54F(0.25)
 C55A(0.43) H55A(0.43) H55B(0.43) H55C(0.43) C55B(0.32) H55D(0.32) H55E(0.32)
 H55F(0.32) C55C(0.25) H55G(0.25) H55H(0.25) H55I(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C32(H32A,H32B), C32(H32C,H32D), C33A(H33A,H33B),
 C33B(H33C,H33D), C34A(H34A,H34B), C34B(H34C,H34D), C42(H42A,H42B), C42(H42C,
 H42D), C43A(H43A,H43B), C43B(H43C,H43D), C44A(H44A,H44B), C44B(H44C,H44D),
 C52(H52A,H52B), C52(H52E,H52F), C52(H52C,H52D), C53A(H53A,H53B), C53B(H53C,
 H53D), C53C(H53E,H53F), C54A(H54A,H54B), C54B(H54C,H54D), C54C(H54E,H54F)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C17(H17), C18(H18), C20(H20), C21(H21),
 C27(H27), C28(H28), C30(H30), C31(H31), C37(H37), C38(H38), C40(H40), C41(H41),
  C47(H47), C48(H48), C50(H50), C51(H51)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C35A(H35A,H35B,H35C), C35B(H35D,
 H35E,H35F), C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C55A(H55A,H55B,H55C),
 C55B(H55D,H55E,H55F), C55C(H55G,H55H,H55I)
;
_shelx_res_checksum              94094
_shelx_fab_checksum              82851
_olex2_exptl_crystal_mounting_method 'CryoLoop with inert mineral oil'
_olex2_submission_original_sample_id sh398
_olex2_submission_special_instructions 'No special instructions were received'