Trisiloxane-centred metal‒organic frameworks and hydrogen bonded assemblies
Delmas, Luke C.; White, Andrew J. P.; Pugh, David; Horton, Peter N.; Coles, Simon J.; Lickiss, Paul D.; Davies, Robert P.; CrystEngComm 20 (2018) 4541–; doi:10.1039/C8CE00662H

data_7231279
_publ_section_title
;
 Trisiloxane-centred metal--organic frameworks and hydrogen bonded
 assemblies
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4541
_journal_paper_doi               10.1039/C8CE00662H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'0.25(C233.65 H254.52 Mn12 N19.22 O75.22 Si12), 5.2(C3 H7 N O)'
_chemical_formula_sum            'C74 H100 Mn3 N10 O24 Si3'
_chemical_formula_weight         1762.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.04 svn.r3437 for OlexSys, GUI svn.r5361)
;
_audit_update_record
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.476(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9725(6)
_cell_length_b                   19.7061(5)
_cell_length_c                   25.3721(5)
_cell_measurement_reflns_used    16467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3360
_cell_measurement_theta_min      2.1480
_cell_volume                     9382.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -52.00  73.00   1.00   65.00    --  -16.70  57.00-120.00  125
  2  \w   -106.00  22.00   1.00   65.00    --  -16.70 -72.00  60.00  128
  3  \w    -50.00  73.00   1.00   65.00    --  -16.70  38.00-180.00  123
  4  \w    -52.00  73.00   1.00   65.00    --  -16.70  57.00 150.00  125
  5  \w    -50.00  10.00   1.00   65.00    --  -16.70  38.00  30.00   60
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139260000
_diffrn_orient_matrix_UB_12      -0.0326255000
_diffrn_orient_matrix_UB_13      0.0043165000
_diffrn_orient_matrix_UB_21      -0.0305417000
_diffrn_orient_matrix_UB_22      0.0151980000
_diffrn_orient_matrix_UB_23      0.0081234000
_diffrn_orient_matrix_UB_31      -0.0174661000
_diffrn_orient_matrix_UB_32      -0.0007052000
_diffrn_orient_matrix_UB_33      -0.0266920000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            59568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       cone
_exptl_crystal_F_000             3692
_exptl_crystal_recrystallization_method
'The material was crystallised from DMF and acetic acid'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10752
_refine_ls_number_restraints     1938
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0833
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             10752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00662h2.cif
_cod_data_source_block           IMP20
_cod_depositor_comments
'Adding full bibliography for 7231278--7231280.cif.'
_cod_database_code               7231279
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44H30 O14 Si3 Mn3 (C3H7NO)8'
_chemical_oxdiff_usercomment     LD_TS_Mn_AcOH(cone)
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O41, N41, C41, C42, C43}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O231, N231, C231, C232, C233}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O241, N241, C241, C242, C243}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O91, N91, C91, C92, C93}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O261, N261, C261, C262, C263}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O51, N51, C51, C52, C53}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O251, N251, C251, C252, C253}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O61, N61, C61, C62, C63}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O71, N71, C71, C72, C73}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O81, N81, C81, C82, C83}
6. Others
 1*[Sof(O71)+Sof(N71)+Sof(C71)+Sof(H71)+Sof(C72)+Sof(H72A)+Sof(H72B)+Sof(H72C)+
 Sof(C73)+Sof(H73A)+Sof(H73B)+Sof(H73C)]+1*[Sof(O81)+Sof(N81)+Sof(C81)+Sof(H81)+
 Sof(C82)+Sof(H82A)+Sof(H82B)+Sof(H82C)+Sof(C83)+Sof(H83A)+Sof(H83B)+Sof(H83C)]+
 1*[Sof(O91)+Sof(N91)+Sof(C91)+Sof(H23D)+Sof(C92)+Sof(H92A)+Sof(H92B)+Sof(H92C)+
 Sof(C93)+Sof(H93A)+Sof(H93B)+Sof(H93C)]=1 with esd of 0.000001
 Sof(O241)=Sof(N241)=Sof(C241)=Sof(H241)=Sof(C242)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C243)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(O41)=Sof(N41)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(O51)=Sof(N51)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=1-FVAR(2)
 Sof(O251)=Sof(N251)=Sof(C251)=Sof(H251)=Sof(C252)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C253)=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(2)
 Sof(O261)=Sof(N261)=Sof(C261)=Sof(H261)=Sof(C262)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C263)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(3)
 Sof(O61)=Sof(N61)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(3)
 Sof(O231)=Sof(N231)=Sof(C231)=Sof(H231)=Sof(C232)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C233)=Sof(H23E)=Sof(H23F)=Sof(H23G)=1-FVAR(4)
 Sof(O31)=Sof(N31)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(4)
 Sof(O71)=Sof(N71)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(5)
 Sof(O81)=Sof(N81)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(6)
 Sof(O91)=Sof(N91)=Sof(C91)=Sof(H23D)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(7)
7.a Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C232(H23A,H23B,H23C), C233(H23E,H23F,H23G), C242(H24A,H24B,H24C),
 C243(H24D,H24E,H24F), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C262(H26A,H26B,
 H26C), C263(H26D,H26E,H26F), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C252(H25A,H25B,H25C), C253(H25D,H25E,H25F), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21), C31(H31), C41(H41), C231(H231),
 C241(H241), C91(H23D), C261(H261), C51(H51), C251(H251), C61(H61), C71(H71),
 C81(H81)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              68029
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id LD_TS_Mn_AcOH
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.249
_oxdiff_exptl_absorpt_empirical_full_min 0.569