Self-assembly of a fac-Mn(CO)3-core containing dinuclear metallacycles using flexible ditopic linkers.
Karthikeyan, S.; Nagarajaprakash, R.; Satheesh, Garisekurthi; Ashok Kumar, Chowan; Manimaran, Bala; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17389–17398; doi:10.1039/c5dt01866h

data_7036345
_publ_section_title
;
 Self-assembly of a fac-Mn(CO)3-core containing dinuclear metallacycles
 using flexible ditopic linkers.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17389
_journal_page_last               17398
_journal_paper_doi               10.1039/c5dt01866h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C34.04 H24 Br2.04 Mn2 N4 O14.04, 2(C H2 Cl2), 2(C H0.75 Cl2)'
_chemical_formula_sum            'C38 H29 Br2 Cl8 Mn2 N4 O14'
_chemical_formula_weight         1318.95
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-14 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.932(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5491(4)
_cell_length_b                   13.3073(7)
_cell_length_c                   15.8423(6)
_cell_measurement_reflns_used    6080
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2013
_cell_measurement_theta_min      2.7100
_cell_volume                     2517.06(19)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   36.00   95.00   1.0000    4.1700
omega____ theta____ kappa____ phi______ frames
    -       19.2928  179.0000    0.0000 59

  2 omega   -1.00   70.00   1.0000    4.1700
omega____ theta____ kappa____ phi______ frames
    -       19.2928   52.0000   48.0000 71

  3 omega  -11.00   19.00   1.0000    4.1700
omega____ theta____ kappa____ phi______ frames
    -       19.2928   90.0000  -41.0000 30

  4 omega   35.00   68.00   1.0000    4.1700
omega____ theta____ kappa____ phi______ frames
    -       19.2928  179.0000  -90.0000 33

  5 omega  -20.00   41.00   1.0000    4.1700
omega____ theta____ kappa____ phi______ frames
    -       19.2928  -37.0000   30.0000 61
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0350409000
_diffrn_orient_matrix_UB_12      0.0075719000
_diffrn_orient_matrix_UB_13      -0.0270508000
_diffrn_orient_matrix_UB_21      0.0242375000
_diffrn_orient_matrix_UB_22      -0.0480820000
_diffrn_orient_matrix_UB_23      0.0123163000
_diffrn_orient_matrix_UB_31      -0.0413854000
_diffrn_orient_matrix_UB_32      -0.0217409000
_diffrn_orient_matrix_UB_33      -0.0364737000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10527
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.375
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+4.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                3289
_reflns_number_total             4417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01866h2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7036343--7036345.cif.'
_cod_original_cell_volume        2517.06(18)
_cod_database_code               7036345
_chemical_oxdiff_formula         'C48 H34 O14 N4 Br2 Mn2'
_chemical_oxdiff_usercomment     '150 K, ORANGE, BLOCK'
_reflns_odcompleteness_completeness 99.83
_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
2. Restrained distances
 Mn1-C17 = Mn1-C17'
 1.797 with sigma of 0.01
 C17-O7 = C17'-O7'
 1.154 with sigma of 0.01
 Mn1-Br1'
 2.532 with sigma of 0.01
 Mn1-O7'
 2.94 with sigma of 0.01
 Cl0A-C19
 1.852 with sigma of 0.02
 Cl2-C19
 1.102 with sigma of 0.02
 Cl1A-C19
 2.102 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C17')
Uanis(O7) = Uanis(O7')
Uanis(Br1) = Uanis(Br1')
Uanis(Cl1) = Uanis(Cl0A) = Uanis(Cl1A) = Uanis(Cl2)
4. Others
 Sof(Br1)=Sof(C17)=Sof(O7)=FVAR(1)
 Sof(Br1')=Sof(O7')=Sof(C17')=FVAR(2)
 Sof(Cl0A)=Sof(Cl1A)=1-FVAR(3)
 Sof(H19A)=Sof(H19B)=Sof(Cl1)=Sof(Cl2)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C18(H18A,H18B), C19(H19A,H19B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'