Facile synthesis of one-dimensional organometallic-organic hybrid polymers based on a diphosphorus complex and flexible bipyridyl linkers.
Elsayed Moussa, M.; Attenberger, B.; Peresypkina, E. V.; Fleischmann, M.; Balázs, G; Scheer, M.; Chemical communications (Cambridge, England) 52 (2016) 10004–10007; doi:10.1039/c6cc05224j

data_7124858
_publ_section_title
;
 Facile synthesis of one-dimensional organometallic-organic hybrid
 polymers based on a diphosphorus complex and flexible bipyridyl linkers.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10004
_journal_page_last               10007
_journal_paper_doi               10.1039/c6cc05224j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C52 H44 Cu2 Mo4 N4 O8 P4, 2(B F4), 0.6(C2 H3 N), 1.98(C H2 Cl2)'
_chemical_formula_sum
'C55.18 H49.76 B2 Cl3.96 Cu2 F8 Mo4 N4.6 O8 P4'
_chemical_formula_weight         1854.04
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-21 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.2466(4)
_cell_length_b                   13.2466(4)
_cell_length_c                   38.4491(11)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      73.2860
_cell_measurement_theta_min      3.4200
_cell_volume                     5842.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -68.00   25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.3256   57.0000    0.0000 93

  2 omega   37.00   99.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000    0.0000 62

  3 omega   68.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   60.0000 110

  4 omega   36.00   99.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   60.0000 63

  5 omega -113.00  -20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.3256  -57.0000 -150.0000 93

  6 omega   22.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       44.3256   37.0000    0.0000 93

  7 omega   33.00  121.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  -90.0000 88

  8 omega   68.00   83.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000 -180.0000 15
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0301613000
_diffrn_orient_matrix_UB_12      -0.0461029000
_diffrn_orient_matrix_UB_13      0.0375233000
_diffrn_orient_matrix_UB_21      -0.1237436000
_diffrn_orient_matrix_UB_22      -0.0914134000
_diffrn_orient_matrix_UB_23      -0.0117355000
_diffrn_orient_matrix_UB_31      0.0427382000
_diffrn_orient_matrix_UB_32      -0.0868099000
_diffrn_orient_matrix_UB_33      -0.0075395000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            22529
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.141
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.311
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             2737
_exptl_crystal_size_max          0.1616
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.0353
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 1890 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7682
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0636
_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^)+(0.1287P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                5859
_reflns_number_total             7682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05224j2.cif
_cod_data_source_block           ems_194_hp_abs
_cod_original_cell_volume        5842.9(4)
_cod_original_formula_sum
'C55.18 H49.76 B2 Cl3.96 Cu2 F8 Mo4 N4.60 O8 P4'
_cod_database_code               7124858
_chemical_oxdiff_formula         C55.2H49.8B2Cl4Cu2F8Mo4N4.6O8P4
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 Cl1-C101 = Cl2-C101
 1.72 with sigma of 0.02
 Cl3-C102 = Cl4-C102
 1.72 with sigma of 0.02
 Cl6-C103 = Cl7_$1-C104_$1 = Cl8_$1-C104_$1 = Cl5-C103
 1.72 with sigma of 0.02
 Cl9-C105 = Cl10-C105
 1.72 with sigma of 0.02
 N100-C200
 1.15 with sigma of 0.02
 C201-C200
 1.5 with sigma of 0.02
 Cl11-C106 = Cl12-C106
 1.72 with sigma of 0.02
 Cl2-Cl1
 2.92 with sigma of 0.04
 Cl7-Cl8
 2.92 with sigma of 0.04
 Cl3-Cl4
 2.92 with sigma of 0.04
 Cl6-Cl5
 2.92 with sigma of 0.04
 Cl10-Cl9
 2.92 with sigma of 0.04
 Cl12-Cl11
 2.92 with sigma of 0.04
3. Rigid bond restraints
 C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uiso(B1) = Uiso(B2)
Uiso(C201) = Uiso(C200) = Uiso(N100)
Uiso(C105) = Uiso(C106)
Uiso(C102) = Uiso(C101)
Uiso(Cl10) = Uiso(Cl9)
Uiso(Cl11) = Uiso(Cl12)
5. Others
 Fixed Sof: F3(0.5) F4(0.5) B1(0.5) F5(0.5) F6(0.5) B2(0.5) N100(0.3)
 C200(0.3) C201(0.3) H20C(0.3) H20D(0.3) H20E(0.3) Cl11(0.1) Cl12(0.1)
 C106(0.1) H10A(0.1) H10B(0.1) Cl7(0.23) Cl8(0.23) C104(0.23) H10C(0.23)
 H10D(0.23) Cl5(0.28) Cl6(0.28) C103(0.28) H10E(0.28) H10F(0.28) Cl9(0.1)
 Cl10(0.1) C105(0.1) H10G(0.1) H10H(0.1) Cl1(0.13) Cl2(0.13) C101(0.13)
 H10I(0.13) H10J(0.13) Cl3(0.15) Cl4(0.15) C102(0.15) H10K(0.15) H10L(0.15)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C106(H10A,H10B), C104(H10C,H10D), C103(H10E,
 H10F), C105(H10G,H10H), C101(H10I,H10J), C102(H10K,H10L)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C22(H22), C23(H23),
  C25(H25), C26(H26)
6.c Idealised Me refined as rotating group:
 C201(H20C,H20D,H20E)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id ems_194
_olex2_submission_special_instructions 'No special instructions were received'